CN109281168A - Soluble polyelectrolyte composite and method for flame retardant finishing of protein fiber - Google Patents
Soluble polyelectrolyte composite and method for flame retardant finishing of protein fiber Download PDFInfo
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- CN109281168A CN109281168A CN201811285490.9A CN201811285490A CN109281168A CN 109281168 A CN109281168 A CN 109281168A CN 201811285490 A CN201811285490 A CN 201811285490A CN 109281168 A CN109281168 A CN 109281168A
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- chitosan
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- flame
- retardant
- phytic acid
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 56
- 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 47
- 239000000835 fiber Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 32
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 32
- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 32
- 229920000867 polyelectrolyte Polymers 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims 4
- 229920001661 Chitosan Polymers 0.000 claims abstract description 48
- 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 abstract description 38
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 37
- 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 abstract description 34
- 229940068041 phytic acid Drugs 0.000 claims abstract description 34
- 239000000467 phytic acid Substances 0.000 claims abstract description 34
- 239000007853 buffer solution Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 51
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 45
- 210000002268 wool Anatomy 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 9
- 229940069078 citric acid / sodium citrate Drugs 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 44
- 150000001875 compounds Chemical class 0.000 abstract description 17
- 239000004753 textile Substances 0.000 abstract description 14
- DWAYUNSAAKQFJZ-UHFFFAOYSA-G magnesium;dipotassium;trisodium;dihydrogen phosphate;hydrogen phosphate;dichloride;sulfate Chemical compound [Na+].[Na+].[Na+].[Mg+2].[Cl-].[Cl-].[K+].[K+].OP(O)([O-])=O.OP([O-])([O-])=O.[O-]S([O-])(=O)=O DWAYUNSAAKQFJZ-UHFFFAOYSA-G 0.000 abstract description 12
- 230000002378 acidificating effect Effects 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 229930014626 natural product Natural products 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 229920000742 Cotton Polymers 0.000 description 8
- 239000002253 acid Substances 0.000 description 6
- 239000003610 charcoal Substances 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229920002518 Polyallylamine hydrochloride Polymers 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- -1 cation Compound Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 1
- 206010000369 Accident Diseases 0.000 description 1
- 241000255789 Bombyx mori Species 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].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-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].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-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000014103 egg white Nutrition 0.000 description 1
- 210000000969 egg white Anatomy 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002103 nanocoating Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000015170 shellfish Nutrition 0.000 description 1
- 229940083982 sodium phytate Drugs 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives 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
- D06M13/10—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
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; 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
- D06M13/244—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
- D06M13/282—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 phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; 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
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of soluble poly pentalyte and its to the method for protein fibre flame-proof treatment, belong to finishing functions of textile fabrics technical field.The present invention prepares soluble poly pentalyte flame-retardant system using phytic acid and chitosan under strongly acidic conditions, then phytic acid and chitosan just can generate ionic bond combination on protein fibre surface after buffer solution is handled, and be attached to protein fibre surface.Phytic acid and chitosan flame-retardant composition used is natural products in the present invention, sufficient raw, and prepared compound polyelectrolyte belongs to environmentally friendly flame-retardant system.Present invention process is simple, and process is short, and economic cost is low, prepared fire-retardant protein fibre excellent fireproof performance, and wash durability is good, has broad application prospects.
Description
Technical field
The present invention relates to a kind of soluble poly pentalyte and its to the method for protein fibre flame-proof treatment, belong to
Finishing functions of textile fabrics technical field.
Background technique
The fire as caused by textile combustion occupies great ratio in home fire accident, not only to human life
Property safety causes great threat, and causes seriously to pollute to environment.Therefore, carrying out flame-proof treatment to textile is still one
Important and urgent task.Related researcher develops many fire retardants to improve the flame retardant property of textile, to reduce
The fire risk of textile.Halogen flame has the characteristics that low dense efficient, and productivity effect is high, is widely used in textile
Flame-proof treatment.But there are lasting harm to environment and the ecosystem for halogen flame, thus its application on the textile by
Great limitation is arrived.Therefore, the exploitation of green, nontoxic and renewable fire proofing causes the concern of researcher.
Phytic acid derives from plant tissue, nontoxic, good biocompatibility, renewable, and phosphorus element content is higher, hinders in preparation
It is attracted wide attention in terms of combustion polymer material.Contain phosphate groups in phytate molecule, enables phytic acid and cation
Compound and metal ion combine to form compound, therefore phytic acid is applied to LBL self-assembly system often to prepare intumescent resistance
Fire coating.The raw material chitin of chitosan is widespread in nature in the shell of shellfish.Natural polymer
Seed chitosan biology functionality and compatibility is good, degradability is strong, has weight in industries such as medicine, food, chemical industry and cosmetics
The application wanted.There are nitrogen-containing groups and great amount of hydroxy group in chitosan molecule, therefore chitosan may act as the hair in Intumescent Retardant System
Infusion and carbon forming agent also have received widespread attention in Fire-proof Finishing Agents for Textile field.The method that Laufer etc. passes through LBL self-assembly
Alternately phytic acid and chitosan precipitation are prepared expansion type flame-retardant coatings and improve the flame retardant property of cotton fabric in surface of cotton fabric,
But 30 preferable flame retardant properties of circulation coatings ability providing cotton fabric of research needs (Galina Laufer,
Christopher Kirkland,Alexander B.Morgan,Jaime C.Grunlan.Intumescent
multilayer nanocoating,made with renewable polyelectrolytes,for flame-
retardant cotton.Biomacromolecules,2012,13(9):2843-2848).Chinese invention patent
CN103321044A discloses a kind of flame-retardant pure silk and preparation method thereof, is replaced silk fabric by the method for layer assembly
Be impregnated in sodium phytate and chitosan solution and prepare flame-retardant pure silk, it is by 10 layers and assembled above after real silk fabric obtain compared with
Good flame retardant property and wash durability.Chinese invention patent CN105803784A discloses a kind of using cationic polyelectrolyte
The method that polyallylamine hydrochloride layer assembly phytic acid prepares function cotton fabric, by laminated assembling technology by polyallylamine
Hydrochloride and phytic acid are enriched in cotton fiber surface, by polyaniline in-situ polymerization on cotton fiber surface after multiple coating, so that cotton is knitted
Object has flame retardant property.But laminated assembling technology is related to repeatedly impregnating polyanion and said polycation solution, and process flow is many and diverse,
Strongly limit its industrial applications.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of soluble poly pentalytes and its right
The method of protein fibre flame-proof treatment prepares soluble poly using natural phytic acid and chitosan as poly- anions and canons electrolyte
Pentalyte flame-retardant system uses citric acid as the solvent of chitosan and crosslinking agent, and by compound polyelectrolyte body
System is applied to the flame-proof treatment of protein fibre.This method preparation process is simple, and process is short, prepared fire-retardant protein fibre
Flame retardant effect is excellent, and durability is preferable, has important practical application value.
The first purpose of the invention is to provide a kind of preparation methods of soluble poly pentalyte, including walk as follows
It is rapid:
(1) it dissolves the chitosan in citric acid solution, adjusting solution ph is 1-2, and chitosan solution is prepared；
(2) plant acid solution is slowly added dropwise into chitosan solution, is stirred evenly, obtained the soluble of homogeneous transparent and plant
Acid/Chitosan-polyelectrolyte complex solution.
Further, the concentration of the compound polyelectrolyte anions in solution chitosan is 1-2%, citric acid concentration
For 5-7%.
Further, the compound polyelectrolyte anions phytic acid concentration is 8-12%.
Further, the compound polyelectrolyte solution ph is 1-2.
Further, in step (1), the pH value is adjusted by adding acetic acid.
Further, in step (1), the citric acid is the solvent of chitosan, and during flame-proof treatment, is served as
Crosslinking agent between chitosan and protein fibre.
A second object of the present invention is to provide the soluble poly pentalytes that the method is prepared.
Third object of the present invention is to provide the methods of protein fibre flame-proof treatment, include the following steps:
(1) protein fibre article impregnation is arranged in the solution of the compound polyelectrolyte, drying
Afterwards, it is handled using citric acid/sodium citrate buffer solution, then washes, dries；
(2) protein fibre product is handled several times according to step (1), carries out baking processing, obtains the fire-retardant egg
White matter fiber product.
Further, the protein fibre is wool and/or silk fiber.
Further, in step (1), the citric acid/sodium citrate pH value of buffer solution is 4-6.
Further, in step (2), the treatment process cycle-index is 1-5 times.
Further, in step (2), described bake carries out at 150-160 DEG C, time 2-4min.
Fourth object of the present invention is to provide the fire-retardant protein fibre product that the method is prepared.
The principle of the present invention is: under strongly acidic conditions, the phosphate radical degree of ionization in phytate molecule is small, with cationic shell
Glycan does not combine, and the two is stabilized in the solution；Phosphate radical electricity under faintly acid and neutrallty condition, in phytate molecule
It is big from degree, can with cationic chitosan by electrostatic attraction in conjunction with form compound, be attached to protein fibre surface.It plants
Acid/chitosan system phosphorus rich in, nitrogen and carbon constitutes Intumscent Flame Retardant System, provides for protein fibre excellent
Different flame retardant property.Further, between phytic acid, chitosan, citric acid and protein fibre existing bridging reaction make it is fire-retardant
Protein fibre has preferable durability of fire-retardant, and the reaction is described as follows: (1) ionic bond between phytic acid and protein fibre
In conjunction with；(2) in conjunction with ionic bond of the phytic acid between chitosan；(3) esterification and crosslinking between chitosan and citric acid reacts；(4) lemon
Acid is reacted with the esterification and crosslinking between protein fibre.
The beneficial effects of the present invention are:
The present invention prepares soluble poly pentalyte flame-retardant system using phytic acid and chitosan under strongly acidic conditions,
The flame-retardant system phosphorus and nitrogen content are high, good flame retardation effect.Phytic acid and chitosan just can be in protein fibres after buffer solution is handled
Dimension table face generates ionic bond and combines, and is attached to protein fibre surface.Phytic acid and chitosan flame-retardant composition used is equal in the present invention
For natural products, sufficient raw, prepared compound polyelectrolyte belongs to environmentally friendly flame-retardant system.Work of the present invention
Skill is simple, and process is short, and economic cost is low, prepared fire-retardant protein fibre excellent fireproof performance, and wash durability is good,
It has broad application prospects.
Detailed description of the invention
Fig. 1 is the heat release rate figure of silk fabric in the embodiment of the present invention 1 and 2；
Fig. 2 is the heat release rate figure of wool fabric in the embodiment of the present invention 4.
Specific embodiment
With reference to embodiment, the embodiment of the present invention is furthur described in detail.Following embodiment is used for
Illustrate the present invention, but is not intended to limit the scope of the invention.
Embodiment 1: silk fabric-citric acid-single-steeping
(1) chitosan (2%) first the preparation of soluble poly pentalyte: is dissolved in citric acid (10%) solution
In, adjusting solution ph using acetic acid is 2, and chitosan solution is made.Then isometric phytic acid (24%) solution is slowly added dropwise
It into chitosan solution, and stirs evenly, obtains soluble phytic acid/Chitosan-polyelectrolyte complex system of homogeneous transparent,
Phytic acid concentration is 12% in solution at this time, chitosan concentration 1%, citric acid concentration 5%, solution ph 2.
(2) preparation of flame-retardant silk fabric: silk fabric is soaked in the resulting compound polyelectrolyte solution of step (1)
Excessive moisture is rolled after stain 10min, pick-up 100% dries silk fabric at 70 DEG C.Then by silk fabric in pH
5min is handled in 6 citric acid/sodium citrate buffer solutions, then washes, dried at 70 DEG C, bake 4min at 150 DEG C, obtain
To flame-retardant silk product.
Embodiment 2: the silk fabric-dipping of citric acid-five times
(1) chitosan (4%) first the preparation of soluble poly pentalyte: is dissolved in citric acid (12%) solution
In, adjusting solution ph using acetic acid is 1, and chitosan solution is made.Then isometric phytic acid (20%) solution is slowly added dropwise
It into chitosan solution, and stirs evenly, obtains soluble phytic acid/Chitosan-polyelectrolyte complex system of homogeneous transparent,
Phytic acid concentration is 10% in solution at this time, chitosan concentration 2%, citric acid concentration 6%, solution ph 1.
(2) preparation of flame-retardant silk fabric: silk fabric is soaked in the resulting compound polyelectrolyte solution of step (1)
Excessive moisture is rolled after stain 10min, pick-up 100% dries silk fabric at 70 DEG C.Then by silk fabric in pH
5min is handled in 5 citric acid/sodium citrate buffer solutions, then washes, dried at 70 DEG C.Above-mentioned steps are repeated 5 times, then at
2min is baked at 160 DEG C, obtains flame-retardant silk product.
Embodiment 3: the silk fabric-dipping of hydrochloric acid-five times
(1) chitosan (4%) first the preparation of soluble poly pentalyte: is dissolved in the hydrochloric acid solution that pH value is 1
In, chitosan solution is made.Then isometric phytic acid (20%) solution is slowly added dropwise into chitosan solution, and stirred equal
It is even, soluble phytic acid/Chitosan-polyelectrolyte complex system of homogeneous transparent is obtained, phytic acid concentration is in solution at this time
10%, chitosan concentration 2%, solution ph 1.
(2) preparation of flame-retardant silk fabric: silk fabric is soaked in the resulting compound polyelectrolyte solution of step (1)
Excessive moisture is rolled after stain 10min, pick-up 100% dries silk fabric at 70 DEG C.Then by silk fabric in pH
5min is handled in 5 citric acid/sodium citrate buffer solutions, then washes, dried at 70 DEG C.Above-mentioned steps are repeated 5 times, then at
2min is baked at 160 DEG C, obtains flame-retardant silk product.
Embodiment 4: the wool fabric-dipping of citric acid-five times
(1) chitosan (4%) first the preparation of soluble poly pentalyte: is dissolved in citric acid (12%) solution
In, adjusting solution ph using acetic acid is 1.3, and chitosan solution is made.Then isometric phytic acid (20%) solution is slowly dripped
It adds in chitosan solution, and stirs evenly, obtain soluble phytic acid/Chitosan-polyelectrolyte complex body of homogeneous transparent
System, phytic acid concentration is 10% in solution at this time, chitosan concentration 2%, citric acid concentration 6%, solution ph 1.3.
(2) preparation of flame resistant wool fabric: wool fabric is soaked in the resulting compound polyelectrolyte solution of step (1)
Excessive moisture is rolled after stain 10min, pick-up 100% dries wool fabric at 70 DEG C.Then by wool fabric in pH
5min is handled in 4 citric acid/sodium citrate buffer solutions, then washes, dried at 70 DEG C.Above-mentioned steps are repeated 5 times, then at
2min is baked at 160 DEG C, obtains flame resistant wool product.
Flame retardant property and water-wash resistance to flame resistant wool and silk fabric can be carried out test.
The limit oxygen index (LOI) of fabric is marked according to GB/T 5454-1997 " textile combustion performance test oxygen index method "
Quasi- measurement.The charcoal of fabric is long, and according to GB/T 5455-2014, " textile combustion performance vertical direction char length glows and afterflame
The measurement of time " standard test.The combustibility of fabric is according to GB/T17591-2006 " flame-retardant textile " standard rating.
The method for washing of flame-retardant textile is referring to GB/T 3921-2008 " textile color stability test fastness to soaping " standard
It carries out, using detergent for silk and wool 2g/L, bath raio 1:50, washing 30min is primary at 40 DEG C.Repetition is washed to required washing times.
The heat release rate of fabric is according to ASTM D7309 (method A) in the miniature calorimeter of FTT0001 (FTT company of Britain)
Upper test.
It is long that table 1 show the LOI and charcoal of flame-retardant silk and wool fabric after different washing times.Silk and sheep are not arranged
The LOI of wool fabric is respectively 24.8% and 23.6%, equal completely burned during vertical combustion, and a length of 30cm of charcoal shows not
Arrange the poor flame retardant properties of silk and wool fabric.The LOI of silk fabric is after a compound polyelectrolyte system arranges
29.1%, long charcoal is about 14.0cm, shows that the flame retardant property of flame-retardant silk fabric is preferable.Through five compound polyelectrolyte systems
The flame retardant property of silk fabric further increases after arrangement, and LOI is still greater than 28.8% after 10 washings, in vertical combustion
In test process can self-extinguishment, charcoal is long to be lower than 15.0cm, meets B1Grade flame retardant property requirement.According to table 1, sorting wool is knitted
Object also has good flame retardant property and wash durability.Embodiment 3 uses dissolving acid agent of the hydrochloric acid as chitosan, arranges silkworm
The flame retardant property of silk fabrics is preferable, but flame retardant property is substantially reduced after washing 5 times, and charcoal is long more than 15.0cm after washing 10 times, no
It can show that the wash durability of flame-retardant silk fabric is poor by vertical burn test.The above results show the crosslinking of citric acid
Effect helps to improve wash durability of the poly- electrolysis compound of phytic acid/chitosan on silk and wool fabric.Through phytic acid/shell
The silk and wool fabric that the poly- electrolysis compound of glycan arranges have good flame retardant property and durability.
Fig. 1 and Fig. 2 show above-mentioned silk and wool fabric heat release rate figure.Silk and wool fabric are through phytic acid/shell
Heat release rate is substantially reduced after glycan compound polyelectrolyte system arranges, and shows the reduction of its fire risk.
The flame retardant property of 1 flame-retardant silk of table and wool fabric after the washing of different numbers
The above case study on implementation illustrates that fibre has excellent in the albumen prepared with soluble poly pentalyte
Flame retardant effect and good durability of fire-retardant.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (10)
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| CN201811285490.9A CN109281168B (en) | 2018-10-31 | 2018-10-31 | Soluble polyelectrolyte composite and method for flame retardant finishing of protein fiber |
| PCT/CN2018/113697 WO2020087503A1 (en) | 2018-10-31 | 2018-11-02 | Soluble polyelectrolyte complex and method for flame-retardant finishing of protein fibers using soluble polyelectrolyte complex |
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| CN109371670A (en) * | 2018-10-29 | 2019-02-22 | 南通纺织丝绸产业技术研究院 | Flame retardant silk and its preparation method and application |
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| CN109281168B (en) | 2020-05-01 |
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