CN116397438A - Durable flame-retardant polyester/cotton blended fabric and preparation method thereof - Google Patents
Durable flame-retardant polyester/cotton blended fabric and preparation method thereof Download PDFInfo
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- CN116397438A CN116397438A CN202310240645.1A CN202310240645A CN116397438A CN 116397438 A CN116397438 A CN 116397438A CN 202310240645 A CN202310240645 A CN 202310240645A CN 116397438 A CN116397438 A CN 116397438A
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- blended fabric
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- 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 180
- 239000003063 flame retardant Substances 0.000 title claims abstract description 180
- 229920000742 Cotton Polymers 0.000 title claims abstract description 126
- 239000004744 fabric Substances 0.000 title claims abstract description 116
- 229920000728 polyester Polymers 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 22
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 claims abstract description 16
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 14
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- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 14
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- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 30
- 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
- 238000000034 method Methods 0.000 claims description 17
- RLHGFJMGWQXPBW-UHFFFAOYSA-N 2-hydroxy-3-(1h-imidazol-5-ylmethyl)benzamide Chemical compound NC(=O)C1=CC=CC(CC=2NC=NC=2)=C1O RLHGFJMGWQXPBW-UHFFFAOYSA-N 0.000 claims description 10
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- 238000004132 cross linking Methods 0.000 abstract description 24
- 230000000694 effects Effects 0.000 abstract description 7
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- 238000009988 textile finishing Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 21
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
- 238000005406 washing Methods 0.000 description 12
- 229910019142 PO4 Inorganic materials 0.000 description 10
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 125000003700 epoxy group Chemical group 0.000 description 6
- 230000032050 esterification Effects 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 239000004254 Ammonium phosphate Substances 0.000 description 5
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 5
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical group [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 description 5
- 235000019289 ammonium phosphates Nutrition 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000003431 cross linking reagent Substances 0.000 description 5
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
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- 230000008569 process Effects 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
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- 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 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
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- 235000002949 phytic acid Nutrition 0.000 description 3
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- 230000002195 synergetic effect Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910014033 C-OH Inorganic materials 0.000 description 2
- 229910014570 C—OH Inorganic materials 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 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 description 2
- 229920004933 Terylene® Polymers 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 150000003077 polyols Chemical group 0.000 description 2
- 238000007142 ring opening reaction Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910014572 C—O—P Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 244000178289 Verbascum thapsus Species 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- -1 phytic acid ammonium salt Chemical class 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
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- 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
- D06M13/44—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 containing nitrogen and phosphorus
- D06M13/453—Phosphates or phosphites containing nitrogen atoms
-
- 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
- D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts thereof
-
- 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
- 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
- D06M2101/06—Vegetal fibres cellulosic
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- 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
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a durable flame-retardant polyester/cotton blended fabric and a preparation method thereof, belonging to the technical field of textile finishing. The preparation method comprises the following steps that (1) tris (epoxypropyl) isocyanurate reacts with pentaerythritol for 3 to 4 hours at 140 to 150 ℃, and then phosphoric acid is added to continue to react for 3 to 4 hours at 115 to 125 ℃ to obtain a reactive flame retardant; (2) Dissolving a reactive flame retardant, polycarboxylic acid, sodium hypophosphite and dicyandiamide in water, and regulating the pH to 7-8 to obtain a flame retardant finishing liquid; (3) And (3) dipping the polyester/cotton blended fabric into the flame-retardant finishing liquid, and performing padding, pre-baking and baking treatment to obtain the durable flame-retardant polyester/cotton blended fabric. The reactive flame retardant is favorable for forming expanded carbon residue on the surface of the polyester/cotton blended fabric, and has the effect of isolating heat, oxygen and combustible gas. The reactive flame retardant is grafted on the polyester/cotton blended fabric in a plurality of crosslinking modes, so that the flame retardant polyester/cotton blended fabric has higher durable flame retardant property.
Description
Technical Field
The invention belongs to the technical field of textile finishing, and particularly relates to a durable flame-retardant polyester/cotton blended fabric and a preparation method thereof.
Background
The polyester/cotton blended fabric has very good performance, has the characteristics of hygroscopicity and heat resistance of pure cotton fabrics, and high elasticity, wear resistance, stiffness and the like of polyester fabrics, and is widely applied to the fields of clothing, indoor home furnishings, decoration, vehicle decoration and the like. However, the polyester/cotton blended fabric has a candlewick effect, so that the flammability is very high, once the fire is caught, the fire is spread easily, and the difficulty of flame-retardant finishing is far greater than that of pure cotton and pure polyester fabrics. Up to now, a great deal of research is carried out on the flame retardant finishing of the polyester/cotton blended fabrics at home and abroad, but no mature commercial durable flame retardant finishing process exists yet.
Reference 1 (study of flame retardant properties of polyester-cotton blended curtain fabrics [ J ]. Chengdu textile high-grade specialty school journal 2016,33 (3): 94-97.) adopts phosphorus-nitrogen composite flame retardant NHPT, resin and the like to carry out durable finishing on polyester-cotton blended fabrics; reference 2 (application of novel flame retardant in polyester-cotton blended fabric [ J ]. Dyeing and finishing technique, 2021,43 (10): 25-28.) adopts the combination of flame retardant for polyester and flame retardant for cotton to improve the flame retardant property of the double-component fabric of the polyester/cotton blended fabric; chinese patent No. 104746338A discloses a flame-retardant working solution and a flame-retardant finishing method for pure cotton fabrics and/or polyester-cotton blended fabrics using the same, wherein the flame-retardant finishing solution is prepared by mixing cotton and polyester fabric flame retardants, and the water-washing resistance of the flame-retardant pure cotton fabrics and the polyester-cotton blended fabrics is improved by adopting N-hydroxymethyl cross-linking agents. The flame retardant and the polyester/cotton blended fabric are subjected to covalent crosslinking to improve the durable flame retardant performance of the flame retardant polyester/cotton blended fabric. However, the N-methylol cross-linking agent adopted by the flame-retardant polyester/cotton blended fabric of the method causes formaldehyde release problem in the finishing and application processes.
Reference 3 (phosphorus/nitrogen flame retardant to the flame retardant finish [ J ]. Textile science report, 2022,43 (6): 94-99,106) adopts phytic acid and urea to synthesize phytic acid ammonium salt, through rolling-baking process to carry out formaldehyde-free flame retardant finish to the terylene/cotton blended fabric, the phytic acid ammonium can produce covalent bond crosslinking with cotton fiber under the catalysis of dicyandiamide, however in the process of baking at high temperature, the ammonium phosphate group is easy to decompose to generate phosphate radical and ammonia gas, resulting in unable to construct phosphorus/nitrogen synergistic flame retardant effect, the flame retardant efficiency of the flame retardant is reduced, the water washing resistance of the finished terylene/cotton blended fabric is poor, and the flame retardant effect is lost after washing.
Therefore, the efficient reactive phosphorus/nitrogen synergistic flame retardant is developed and used for preparing the polyester/cotton blended fabric with excellent flame retardant durability, and has very important significance in the finishing and application processes without formaldehyde release problem.
Disclosure of Invention
In order to solve the technical problems, the invention provides a durable flame-retardant polyester/cotton blended fabric and a preparation method thereof. The cotton fiber component of the polyester/cotton blend fabric is less than that of the pure cotton fabric, so how to efficiently graft the flame retardant on the cotton fiber component, thereby imparting durable flame retardant property to the polyester/cotton blend fabric, is a difficulty. The synthesis integrates various flame retardant groups and various reactive groups, develops the efficient reactive flame retardant, and simultaneously grafts the flame retardant on the polyester/cotton blended fabric in a plurality of crosslinking modes, thereby being beneficial to improving the durable flame retardant performance of the polyester/cotton blended fabric. In addition, the reaction conditions of different reactive groups such as reaction temperature and pH value have great difference, and the compatibility between flame retardant groups is also a difficulty in preparing the multi-reactive group flame retardant.
The first object of the present invention is to provide a method for preparing durable flame retardant polyester/cotton blend fabrics, comprising the steps of,
(1) Reacting tris (epoxypropyl) isocyanurate with pentaerythritol at 140-150 ℃ for 3-4 h, adding phosphoric acid, and continuing to react at 115-125 ℃ for 3-4 h to obtain a reactive flame retardant;
(2) Dissolving the reactive flame retardant, the polybasic carboxylic acid, the sodium hypophosphite and the dicyandiamide in the step (1) in water, and regulating the pH to 7-8 to obtain a flame-retardant finishing liquid;
(3) And (3) dipping the polyester/cotton blended fabric into the flame-retardant finishing liquid in the step (2), and performing padding, pre-baking and baking treatment to obtain the durable flame-retardant polyester/cotton blended fabric.
In one embodiment of the present invention, in the step (1), the reactive flame retardant contains an acid source, an air source and a carbon source, and the combination of the three can effectively construct an intumescent flame retardant, which has higher flame retardant performance; in addition, the flame retardant has various reactive groups, can be crosslinked with polyester/cotton blended fabrics in various crosslinking modes at the same time, and solves the problems of poor grafting efficiency and poor flame retardance durability of single active group. The structure of the reactive flame retardant is as follows:
in one embodiment of the present invention, in step (1), the molar ratio of tris (epoxypropyl) isocyanurate, pentaerythritol, and phosphoric acid is 1:1-1.3:2-2.3. The molar ratio of tris (epoxypropyl) isocyanurate to pentaerythritol is 1:1-1.3, the epoxy group of tri (epoxypropyl) isocyanurate and the hydroxyl of pentaerythritol are subjected to epoxy ring-opening addition reaction, and the excessive pentaerythritol is helpful for improving the reaction efficiency, but is wasted when the amount of pentaerythritol is too high. The molar ratio of tris (epoxypropyl) isocyanurate to phosphoric acid is 1:2-2.3, the two remaining epoxy groups of the tri (epoxypropyl) isocyanurate and the phosphate can undergo an epoxy ring-opening addition reaction, and the phosphoric acid is slightly excessive to help improve the reaction efficiency, but is wasted when the phosphoric acid is excessive.
In one embodiment of the invention, in step (1), the reaction is carried out for 3h to 4h at 140 ℃ to 150 ℃ and 140 ℃ to 150 ℃ is higher than the melting point of tris (epoxypropyl) isocyanurate, and the tris (epoxypropyl) isocyanurate is liquid under the temperature condition, so as to facilitate the reaction; the reaction time is 3-4 h, the rise of the reaction temperature and the extension of the reaction time are helpful for the synthesis reaction, but the waste is caused by too high reaction time.
In one embodiment of the present invention, in step (1), the reaction is continued for 3 to 4 hours at 115 to 125 ℃, and the increase in reaction temperature and the extension of time contribute to the progress of the synthesis reaction, but are wasteful if too high.
In one embodiment of the present invention, in step (1), the method further comprises a step of purifying the reactive flame retardant, specifically comprising: the phosphate flame retardant is dried in vacuum firstly, then methanol and toluene are adopted for purification, and the yield of the reactive flame retardant is 74-77%.
In one embodiment of the invention, in step (2), the polycarboxylic acid is 1,2,3, 4-butanetetracarboxylic acid and/or citric acid.
In one embodiment of the invention, in step (2), the concentration of the reactive flame retardant in the flame retardant finishing liquid is 100g/L to 200g/L. The increase of the consumption of the reactive flame retardant is helpful for improving the flame retardant property of the polyester/cotton blended fabric, but the content of the flame retardant on the polyester/cotton blended fabric can reach saturation, and excessive flame retardant is wasted.
In one embodiment of the present invention, in step (2), the molar ratio of the reactive flame retardant to the polycarboxylic acid is 1:1.3-1.5; the mass of dicyandiamide is 5% -10% of that of the reactive flame retardant; the mass of the sodium hypophosphite is 40-50% of that of the polycarboxylic acid.
In one embodiment of the invention, in step (2), the pH adjustor is aqueous ammonia, at which pH conditions the phosphate groups are converted to ammonium phosphate groups, facilitating covalent bond cross-linking with the cotton fibers.
In one embodiment of the present invention, in the step (3), the post-padding rolling reduction is 100% -110%. The higher the rolling surplus rate is, the higher the liquid carrying amount of the polyester/cotton blended fabric is, which is favorable for improving the flame retardant property, but the content of the flame retardant on the fabric with too high content can reach saturation, so that the waste is caused.
In one embodiment of the present invention, in the step (3), the pre-baking temperature is 70 ℃ to 80 ℃ for 2min to 4min; the baking temperature is 160-170 ℃ and the baking time is 3-5 min. The baking temperature is raised to facilitate the esterification and crosslinking reaction between the ammonium phosphate group of the reactive flame retardant and the hydroxyl groups of the cotton fibers, and the esterification and crosslinking reaction between the polycarboxylic acid, the reactive flame retardant and the cotton fibers, but the excessive heating is wasteful and the physical properties of the fabric are easily damaged.
In one embodiment of the present invention, in step (3), the polyester/cotton blend fabric is a 35/65, 40/60 or 45/55 polyester/cotton blend fabric.
In one embodiment of the invention, the ammonium phosphate group of the reactive flame retardant can be subjected to esterification crosslinking reaction with the hydroxyl groups of the cotton fiber under the catalysis of dicyandiamide; the polycarboxylic acid serving as a cross-linking agent can perform esterification reaction with the hydroxyl groups of the reactive flame retardant and the hydroxyl groups of the cotton fibers, so that the reactive flame retardant can be grafted on the polyester/cotton blended fabric through covalent bonds; the slightly excessive polycarboxylic acid is helpful for improving the crosslinking efficiency, and the excessive polycarboxylic acid is wasted; sodium hypophosphite is used as a catalyst to promote the carboxyl of the polycarboxylic acid and the hydroxyl of the reactive flame retardant and cotton fiber to generate esterification and crosslinking reaction.
The second object of the invention is to provide a durable flame-retardant polyester/cotton blended fabric prepared by the method.
In one embodiment of the present invention, the flame retardant properties of the durable flame retardant polyester/cotton blend fabric are: limiting Oxygen Index (LOI) is 29.5-32.8%, damage length is 11.5-8.9cm, no molten drop is generated (LOI of unmodified polyester/cotton blended fabric is 17.3%, damage length is 30 cm); the flame-retardant/cotton blended fabric finished by 200g/L of flame retardant can resist 40 times of water washing, which shows that the modified polyester fabric has high-efficiency durable flame-retardant function.
The principle of the invention is as follows:
the invention combines active hydroxyl and phosphate radical into a whole by adopting tri (epoxypropyl) isocyanurate as an intermediate, contains a nitrogen-containing heterocyclic flame-retardant radical, and is organically combined with a phosphorus-containing flame-retardant radical to construct a phosphorus/nitrogen synergistic flame-retardant effect, thus having higher flame-retardant efficiency. Catalyzing the esterification reaction of ammonium phosphate and hydroxyl of cotton fiber by dicyandiamide to generate phosphate bond; and meanwhile, polycarboxylic acid is used as a cross-linking agent, the polycarboxylic acid reacts with hydroxyl groups of the flame retardant and hydroxyl groups of cotton fibers, and the flame retardant is fixed on the polyester/cotton blended fabric through covalent bonds in various cross-linking modes, so that a durable flame retardant effect is achieved. The reactive hydroxyl groups and the phosphate groups have similar reaction conditions, and can be crosslinked with the polyester/cotton blended fabric under the high-temperature baking condition. The ammonium phosphate can be subjected to esterification reaction with hydroxyl groups of cotton fibers under the catalysis of dicyandiamide, and in addition, the polybasic carboxylic acid is used as a cross-linking agent between the flame retardant and the cotton fibers to further graft the flame retardant on the polyester/cotton blended fabric, and formaldehyde is not generated by both cross-linking means.
However, when the polyester/cotton blend fabric is grafted by using the hydroxyl group and the ammonium phosphate group of the flame retardant alone, flame retardance durability is poor. This is because when the crosslinking is performed using the ammonium phosphate and the hydroxy/polycarboxylic acid as flame retardants alone, the saturation degree of the flame retardants involved in the crosslinking is low, and a sufficient amount of the flame retardants cannot be grafted onto the polyester/cotton blend fabric through covalent bonds. And the saturation of the crosslinked flame retardant can be improved in a double crosslinking mode, so that more hydroxyl groups participate in the reaction on the cotton fiber. Meanwhile, the flame retardant through double crosslinking has better durability on the polyester/cotton blended fabric because the condition required for simultaneously breaking the covalent bonds of the phosphate and the carboxylate is more severe.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) According to the preparation method, the phosphorus-containing flame retardant group, the nitrogen-containing heterocycle and the polyol group are combined through covalent bonds to synthesize the reactive flame retardant with three groups as a whole, so that nitrogen loss caused by baking is avoided; phosphate in the reactive flame retardant is used as an acid source, nitrogen-containing heterocycle is used as an air source, polyol is used as carbon, and the combination of the three can effectively construct the intumescent flame retardant; in the combustion process, the reactive flame retardant is favorable for forming the expansion type carbon residue on the surface of the polyester/cotton blended fabric, has the effect of isolating heat, oxygen and combustible gas, and has excellent flame retardant property.
(2) According to the preparation method, the reactive flame retardant reacts with ammonia water through ionic bonds to form ammonium phosphate, and under the action of a dicyandiamide catalyst and high temperature, the ammonium phosphate reacts with hydroxyl groups of cotton fibers in an esterification manner; the reactive flame retardant has two phosphate active sites, has higher reactivity with cotton fibers, and reacts with the cotton fibers in the polyester/cotton blended fabric through covalent bonds; in addition, the polycarboxylic acid can also perform esterification crosslinking reaction with the reactive flame retardant and cotton fibers under the condition, and the reactive flame retardant is grafted on the polyester/cotton blended fabric in a plurality of crosslinking modes, so that the flame retardant polyester/cotton blended fabric has higher washing resistance.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings, in which:
FIG. 1 shows a reactive flame retardant in example 1 of the present invention 13 C Nuclear magnetic resonance spectrum
FIG. 2 is a graph of vertical burning test of the non-flame-retardant modified polyester/cotton blend fabric of the present invention, the durable flame-retardant polyester/cotton blend fabric of example 1, after 0 and 40 water washes.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Example 1
A durable flame-retardant polyester/cotton blended fabric and a preparation method thereof specifically comprise the following steps:
(1) Adding 0.1mol of tris (epoxypropyl) isocyanurate into a three-neck flask, heating to 145 ℃, adding 0.12mol of pentaerythritol to react for 3.5 hours, adding 0.22mol of phosphoric acid to continue to react for 3.5 hours at 120 ℃, and purifying by adopting methanol and toluene after vacuum drying to obtain the reactive flame retardant with the yield of 76%.
(2) Dissolving a reactive flame retardant, 1,2,3, 4-butane tetracarboxylic acid, sodium hypophosphite and dicyandiamide in water, adding ammonia water to adjust the pH value of the solution to 8, and obtaining flame-retardant finishing liquid; the concentration of the reactive flame retardant in the flame retardant finishing liquid is 200g/L; the molar ratio of the reactive flame retardant to the 1,2,3, 4-butane tetracarboxylic acid is 1:1.5; the mass of dicyandiamide is 8% of that of the reactive flame retardant; the mass of sodium hypophosphite is 50% of that of 1,2,3, 4-butane tetracarboxylic acid.
(3) Dipping 45/55 polyester/cotton blended fabric into the flame retardant finishing liquid, wherein the padding residual rate is 105% after padding; and pre-baking the polyester/cotton blended fabric for 3min at 75 ℃ and finally baking the polyester/cotton blended fabric for 4min at 165 ℃ to obtain the durable flame-retardant polyester/cotton blended fabric.
Comparative example 1
Essentially the same as in example 1, except that dicyandiamide was not added in step (2), the mono-crosslinking was carried out by 1,2,3, 4-butanetetracarboxylic acid.
Comparative example 2
Essentially the same as in example 1, except that step (2) was carried out without adding 1,2,3, 4-butanetetracarboxylic acid, the single crosslinking was carried out by dicyandiamide.
Example 2
(1) Adding 0.1mol of tris (epoxypropyl) isocyanurate into a three-neck flask, heating to 140 ℃, adding 0.1mol of pentaerythritol for reaction for 4 hours, adding 0.2mol of phosphoric acid for continuous reaction for 4 hours at 115 ℃, and purifying by adopting methanol and toluene after vacuum drying to obtain the reactive flame retardant with the yield of 75 percent.
(2) Dissolving a reactive flame retardant, 1,2,3, 4-butane tetracarboxylic acid, sodium hypophosphite and dicyandiamide in water, adding ammonia water to adjust the pH value of the solution to 7, and obtaining flame-retardant finishing liquid; the concentration of the reactive flame retardant in the flame retardant finishing liquid is 170g/L; the molar ratio of the reactive flame retardant to the 1,2,3, 4-butane tetracarboxylic acid is 1:1.3; the mass of dicyandiamide is 6% of that of the reactive flame retardant; the mass of sodium hypophosphite is 40% of that of 1,2,3, 4-butane tetracarboxylic acid.
(3) Immersing 40/60 polyester/cotton blended fabric into the flame-retardant finishing liquid, wherein the padding residual rate is 110% after padding; and pre-baking the polyester/cotton blended fabric for 4min at 70 ℃ and finally baking the polyester/cotton blended fabric for 5min at 160 ℃ to obtain the durable flame-retardant polyester/cotton blended fabric.
Example 3
(1) Adding 0.1mol of tris (epoxypropyl) isocyanurate into a three-neck flask, heating to 150 ℃, adding 0.13mol of pentaerythritol for reaction for 3 hours, adding 0.23mol of phosphoric acid for continuous reaction for 3 hours at 125 ℃, and purifying by adopting methanol and toluene after vacuum drying to obtain the reactive flame retardant with the yield of 77 percent.
(2) Dissolving a reactive flame retardant, citric acid, sodium hypophosphite and dicyandiamide in water, adding ammonia water to adjust the pH value of the solution to 7.5, and obtaining flame-retardant finishing liquid; the concentration of the reactive flame retardant in the flame retardant finishing liquid is 125g/L; the molar ratio of the reactive flame retardant to the citric acid is 1:1.5; the mass of dicyandiamide is 10% of that of the reactive flame retardant; the mass of the sodium hypophosphite is 45% of that of the citric acid.
(3) Dipping 35/65 polyester/cotton blended fabric into the flame-retardant finishing liquid, wherein the padding residual rate is 100% after padding; and pre-baking the polyester/cotton blended fabric for 2min at 80 ℃ and finally baking the polyester/cotton blended fabric for 3min at 170 ℃ to obtain the durable flame-retardant polyester/cotton blended fabric.
Example 4
(1) Adding 0.1mol of tris (epoxypropyl) isocyanurate into a three-neck flask, heating to 147 ℃, adding 0.12mol of pentaerythritol to react for 3.5 hours, adding 0.21mol of phosphoric acid to continue to react for 3.6 hours at 122 ℃, and purifying by adopting methanol and toluene after vacuum drying to obtain the reactive flame retardant with the yield of 74%.
(2) Dissolving a reactive flame retardant, citric acid, sodium hypophosphite and dicyandiamide in water, adding ammonia water to adjust the pH value of the solution to 7, and obtaining flame-retardant finishing liquid; the concentration of the reactive flame retardant in the flame retardant finishing liquid is 100g/L; the molar ratio of the reactive flame retardant to the citric acid is 1:1.4; the mass of dicyandiamide is 5% of that of the reactive flame retardant; the mass of sodium hypophosphite is 43% of that of citric acid.
(3) Immersing 40/60 of polyester/cotton blended fabric into the flame-retardant finishing liquid, wherein the padding residual rate is 105% after padding; and pre-baking the polyester/cotton blended fabric for 3min at 75 ℃ and finally baking the polyester/cotton blended fabric for 4min at 165 ℃ to obtain the durable flame-retardant polyester/cotton blended fabric.
Test example 1
The reactive flame retardant prepared in example 1 was characterized and the results are shown in FIG. 1. As can be seen from fig. 1, chemical shifts at 151.7 and 150.5ppm are caused by carbon atoms of the c=o structure on the nitrogen heterocycle, chemical shifts at 57.4 and 48.0ppm are caused by carbon atoms of the pentaerythritol C-OH structure and the central carbon atom, and chemical shifts at 45.1ppm are caused by carbon atoms of the C-N structure attached to the epoxy group; the chemical shifts at 66.9ppm and 63.5ppm are caused by the carbon atoms of the C-O-P and C-OH structures formed after the reaction of the epoxy groups in the reactive flame retardant structure, indicating that the epoxy groups are reacted with the phosphate. The chemical shift at 74.8ppm is caused by a carbon atom in the C-O structure after the epoxy group has reacted with the pentaerythritol hydroxyl group. The above structure shows that the reactive flame retardant was successfully synthesized.
Test example 2
The flame retardant properties of the unfinished polyester/cotton blend fabrics, the finished polyester/cotton blend fabrics of examples 1-4 and comparative examples 1-2 were tested.
The Limiting Oxygen Index (LOI) of the fabric is measured according to GB/T5454-1997 standard of the oxygen index method of the Experimental Combustion Performance of textiles.
The carbon residue of the flame-retardant polyester/cotton blended fabric and the non-finished polyester/cotton blended fabric is tested under the nitrogen condition by adopting a thermal analysis test method.
The damage length of the fabric is measured according to GB/T5455-2014 standard of measurement of smoldering and continuous burning time of damage length of vertical direction of burning property of textile.
The burning performance of the fabric is evaluated according to the GB/T17591-2006 flame retardant fabric standard.
The water wash method is described in AATCC61-2006, accelerated test of washing fastness for domestic and commercial applications.
FIG. 2 is a vertical burning test chart of a non-flame-retardant modified polyester/cotton blend fabric, the durable flame-retardant polyester/cotton blend fabric of example 1 after 0 and 40 water washes:
table 1 shows the relevant performance parameters of the final measured polyester/cotton blend fabrics:
TABLE 1
| Sample preparation | LOI/％ | 700 ℃ carbon residue/% | Damage length/cm | Number of water washing resistance |
| Unfinished polyester/cotton blended fabric | 17.3％ | 8.3 | 30 | 0 |
| Example 1 | 32.8 | 35.3 | 8.9 | 40 |
| Comparative example 1 | 32.4 | 34.1 | 9.2 | 10 |
| Comparative example 2 | 32.6 | 34.5 | 9.0 | 15 |
| Example 2 | 31.9 | 30.9 | 9.7 | 35 |
| Example 3 | 30.7 | 26.2 | 10.8 | 30 |
| Example 4 | 29.5 | 22.7 | 11.5 | 25 |
As can be seen from table 1 and fig. 2, the flame retardant properties of the durable flame retardant polyester/cotton blend fabrics are: limiting Oxygen Index (LOI) is 29.5-32.8%, damage length is 11.5-8.9cm, no molten drop is generated (LOI of unmodified polyester/cotton blended fabric is 17.3%, damage length is 30 cm); the flame-retardant/cotton blended fabric finished by 200g/L of the flame retardant can resist 40 times of water washing, which shows that the modified polyester/cotton blended fabric has high-efficiency and durable flame-retardant function. Comparative example 1 was resistant to 10 times of water washing and comparative example 2 was resistant to 15 times of water washing, indicating that the single crosslinking by the reactive flame retardant through the polycarboxylic acid and the polyester/cotton blend fabric, the single crosslinking by the phosphate of the reactive flame retardant and the polyester/cotton blend fabric were poor in both water washing resistance, and the double crosslinking in the examples gave excellent water washing resistance to the polyester/cotton blend fabric.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
1. A preparation method of durable flame-retardant polyester/cotton blended fabric is characterized by comprising the following steps of,
(1) Reacting tris (epoxypropyl) isocyanurate with pentaerythritol at 140-150 ℃ for 3-4 h, adding phosphoric acid, and continuing to react at 115-125 ℃ for 3-4 h to obtain a reactive flame retardant;
(2) Dissolving the reactive flame retardant, the polybasic carboxylic acid, the sodium hypophosphite and the dicyandiamide in the step (1) in water, and regulating the pH to 7-8 to obtain a flame-retardant finishing liquid;
(3) And (3) dipping the polyester/cotton blended fabric into the flame-retardant finishing liquid in the step (2), and performing padding, pre-baking and baking treatment to obtain the durable flame-retardant polyester/cotton blended fabric.
2. The method of producing durable flame retardant polyester/cotton blend fabrics according to claim 1, wherein in step (1), the structure of the reactive flame retardant is as follows:
3. the method of making a durable flame retardant polyester/cotton blend fabric according to claim 1, wherein in step (1), the molar ratio of tris (epoxypropyl) isocyanurate, pentaerythritol and phosphoric acid is 1:1-1.3:2-2.3.
4. The method of producing a durable flame retardant polyester/cotton blend fabric according to claim 1, wherein in step (2), the polycarboxylic acid is 1,2,3, 4-butanetetracarboxylic acid and/or citric acid.
5. The method for producing durable flame retardant polyester/cotton blend fabrics according to claim 1, wherein in the step (2), the concentration of the reactive flame retardant in the flame retardant finishing liquid is 100g/L to 200g/L.
6. The method of producing durable flame retardant polyester/cotton blend fabrics according to claim 1, wherein in step (2), the molar ratio of the reactive flame retardant to the polycarboxylic acid is 1:1.3-1.5; the mass of dicyandiamide is 5% -10% of that of the reactive flame retardant; the mass of the sodium hypophosphite is 40-50% of that of the polycarboxylic acid.
7. The method of producing durable flame retardant polyester/cotton blend fabrics according to claim 1, wherein in step (3), the padding residual ratio after padding is 100% -110%.
8. The method for producing durable flame retardant polyester/cotton blend fabrics according to claim 1, wherein in step (3), the pre-baking temperature is 70 ℃ to 80 ℃ for 2min to 4min; the baking temperature is 160-170 ℃ and the baking time is 3-5 min.
9. The method of making a durable flame retardant polyester/cotton blend fabric according to claim 1, wherein in step (3), the polyester/cotton blend fabric is a 35/65, 40/60 or 45/55 polyester/cotton blend fabric.
10. A durable flame retardant polyester/cotton blend fabric made by the method of any one of claims 1-9.
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