CN116043532A - Flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric and preparation method thereof - Google Patents
Flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric and preparation method thereof Download PDFInfo
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- CN116043532A CN116043532A CN202211304087.2A CN202211304087A CN116043532A CN 116043532 A CN116043532 A CN 116043532A CN 202211304087 A CN202211304087 A CN 202211304087A CN 116043532 A CN116043532 A CN 116043532A
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- sepiolite
- cotton fabric
- hybrid sol
- flame
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- 239000004113 Sepiolite Substances 0.000 title claims abstract description 176
- 229910052624 sepiolite Inorganic materials 0.000 title claims abstract description 176
- 235000019355 sepiolite Nutrition 0.000 title claims abstract description 170
- 229920000742 Cotton Polymers 0.000 title claims abstract description 119
- 239000004744 fabric Substances 0.000 title claims abstract description 108
- 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 75
- 239000003063 flame retardant Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920000728 polyester Polymers 0.000 claims description 60
- 239000006185 dispersion Substances 0.000 claims description 33
- 239000011248 coating agent Substances 0.000 claims description 32
- 238000000576 coating method Methods 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 28
- 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 24
- 229920000805 Polyaspartic acid Polymers 0.000 claims description 22
- 108010064470 polyaspartate Proteins 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 19
- 230000002378 acidificating effect Effects 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- 230000004584 weight gain Effects 0.000 claims description 12
- 235000019786 weight gain Nutrition 0.000 claims description 12
- 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 11
- 235000002949 phytic acid Nutrition 0.000 claims description 11
- 229940068041 phytic acid Drugs 0.000 claims description 11
- 239000000467 phytic acid Substances 0.000 claims description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract description 18
- 239000004753 textile Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229910014033 C-OH Inorganic materials 0.000 description 5
- 229910014570 C—OH Inorganic materials 0.000 description 5
- 229910008051 Si-OH Inorganic materials 0.000 description 5
- 229910006358 Si—OH Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 235000003704 aspartic acid Nutrition 0.000 description 4
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphonic acid group Chemical group P(O)(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009396 hybridization Methods 0.000 description 2
- -1 hydrogen ions Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000007524 organic acids Chemical group 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- 238000012795 verification Methods 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
- 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
- D06M11/77—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 silicon or compounds thereof
- D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic 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
- D06M13/244—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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/59—Polyamides; Polyimides
-
- 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
-
- 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
-
- 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
-
- 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
- D06M2200/50—Modified hand or grip properties; Softening compositions
-
- 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)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a flame-retardant sepiolite-based hybrid sol coated polyester-cotton fabric and a preparation method thereof. The sepiolite-based hybrid sol is coated on the surface of the polyester-cotton fabric, and is pre-baked and then baked to obtain the flame-retardant sepiolite-based hybrid sol coated polyester-cotton fabric, and the step can endow the polyester-cotton fabric with water washing resistance and flame retardance. The sepiolite-based hybrid sol prepared by the method overcomes the defects of small molecular weight and large brittleness of the traditional silica sol prepared by taking silicate as a raw material, has a certain molecular network structure, can form a film with certain flexibility on the surface of a textile, and endows the textile material with flame retardance and certain mechanical property.
Description
Technical Field
The invention belongs to the technical field of hybrid sol-coated polyester-cotton fabric and preparation thereof, and particularly relates to a preparation method of a flame-retardant sepiolite-based organic/inorganic hybrid sol-coated polyester-cotton fabric.
Background
With the progress of society, the performance of various materials is gradually developed, however, the flame retardance of flexible materials is still an important proposition. The blended fabric represented by polyester cotton has wide application range due to various excellent performances, but the performance difference among components is large, the combustion condition is complex, and the flame retardation problem of the material is not completely solved. Based on this, how to reduce the loss of lives and properties of people caused by burning textiles has been the focus of various social circles.
The flame retardant of textile materials began in the 19 th century and developed from temporary flame retardant to semi-durable flame retardant, durable flame retardant according to the flame retardant aging. Flame-retardant finishing methods of textiles are also various, and the common methods are mainly padding and baking methods. The traditional flame-retardant after-finishing of textiles has the defects of exceeding formaldehyde release, non-durable flame-retardant effect, rough hand feeling, reduced mechanical property and the like, and the wide application of flame-retardant textiles in the field of materials is limited.
The traditional preparation of the silica sol mainly uses tetraethyl orthosilicate and absolute ethyl alcohol to react under an acidic condition, so that the silica sol is generated, a flexible coating cannot be formed on the surface of a fabric after the generated sol is dried, the mechanical strength is poor, the silica sol is not suitable for preparing film materials, and flame retardant protection cannot be generated on the textile. The modification of the traditional silica sol mainly adopts small molecules or chain chemical reagents such as methyltriethoxysilane, silane coupling agents with different structures, polyethylene glycol and the like, the main aim is to improve the flexibility, mechanical properties and the like of the silica sol, the flame retardance and other functionalities of the silica sol are not obviously affected, and the combination of the silica sol prepared by the traditional method and textiles needs to adopt functional groups to functionally modify the silica sol, so that the silica sol is endowed with certain chemical activity, complex process and more limiting conditions.
Therefore, a preparation method of a flame-retardant polyester-cotton fabric product which is simple in process, good in flame retardance, environment-friendly and durable is needed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric and a preparation method thereof.
In a first aspect, the invention provides a preparation method of a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric, which comprises the following specific steps:
s1: dispersing sepiolite in water, and stirring to obtain sepiolite dispersion liquid;
s2: mixing the sepiolite dispersion liquid and a bio-based acidic substance and then reacting to prepare sepiolite-based hybrid sol;
s3: and coating the sepiolite-based hybrid sol on the surface of the polyester cotton fabric, and baking after pre-baking to obtain the flame-retardant sepiolite-based hybrid sol coated polyester cotton fabric.
Preferably, the sepiolite is α -sepiolite.
Preferably, the sepiolite dispersion in S1 is obtained by stirring the mixture with a homogenizer at a concentration of 1 to 10g/L.
Preferably, the bio-based acidic substance in S2 is phytic acid or polyaspartic acid.
Preferably, the concentration of the phytic acid solution is 5-15 g/L, and the concentration of the polyaspartic acid solution is 3-10 g/L.
Preferably, the weight ratio of the sepiolite dispersion to the bio-based acidic substance is 0.2 to 1.
Preferably, the sepiolite-based hybrid sol prepared in the step S2 is prepared at a temperature of 25-95 ℃ for 2-24 hours.
Preferably, the weight gain rate of the coating in S3 is 10% to 100%.
Preferably, the pre-baking temperature in the step S3 is 80-100 ℃ and the pre-baking time is 5-10 min; and S3, baking at 130-180 ℃ for 2-10 min.
In a second aspect, the present application provides a flame retardant sepiolite-based hybrid sol coated polyester cotton fabric prepared using the method of the first aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) The sepiolite is used as a raw material, mg atoms in a magnesium oxide octahedron in a sepiolite three-dimensional framework structure are dissolved out under an acidic condition, the three-dimensional framework structure is converted into an amorphous silica sol material, active groups in an organic acid structure react with Si-OH in the silica sol structure in the conversion process, the sol is modified, the sepiolite-based hybrid sol with certain mechanical properties is prepared, and the sol is applied to the field of flame retardance of polyester cotton fabrics for the first time;
(2) According to the invention, sepiolite is used as a raw material, functional groups in the prepared sepiolite-based hybrid silica sol structure are more, for example, si-OH in the silica sol can generate hydrogen bond action with C-OH on the surface of cotton fiber in polyester cotton fabric, phosphonate in the phytic acid structure can generate hydrogen bond or covalent bond with C-OH on the surface of cotton fiber, and-NH-, -C=O in the polyaspartic acid structure can generate hydrogen bond action with C-OH on the surface of cotton fiber, so that the coating fastness of the silica sol to the textile is improved, the process is simple, the energy consumption is lower, and the method can be used for industrial production;
(3) The sepiolite-based hybrid sol prepared by taking sepiolite as a raw material and phytic acid and polyaspartic acid as acid auxiliary agents is coated on the surface of polyester-cotton fabric in a coating mode, the main component of the sol is silica sol, other auxiliary agents are biological-based environment-friendly materials, and the problem of formaldehyde release is avoided; the sepiolite-based hybrid sol has certain flexibility, and the coated textile has soft hand feeling and does not influence usability; as different functional groups interact with the groups on the surface of the cotton fiber, and the material still has flame retardance after being washed by flame retardance test verification, the surface of the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric has washability.
Drawings
FIG. 1 is a diagram of the skeleton structure of α -sepiolite;
FIG. 2 is a vertical burning chart of a flame retardant sepiolite-based hybrid sol coated polyester-cotton fabric prepared in each example: wherein fig. 2 (a) is pure polyester cotton; FIG. 2 (b) is sample C prepared in example 3; FIG. 2 (c) is sample B prepared in example 2; FIG. 2 (D) is a sample D prepared in example 4; FIG. 2 (e) is sample A prepared in example 1;
FIG. 3 is a vertical burning graph of a pure polyester cotton sample CK (FIG. 3 a) and a flame retardant sepiolite-based hybrid sol coated polyester cotton fabric sample A-1 (FIG. 3 b) after water washing.
Fig. 4 is a flowchart of the preparation of the flame retardant sepiolite-based hybrid sol coated polyester-cotton fabric provided by the invention.
Detailed Description
The invention is further illustrated and described below with reference to the drawings and detailed description. The technical features of the embodiments of the invention can be combined correspondingly on the premise of no mutual conflict.
As shown in fig. 4, the invention provides a preparation method of a flame retardant sepiolite-based hybrid sol coated polyester-cotton fabric, which comprises the following steps:
(1) Sepiolite is dispersed in water, a homogenizer is adopted to uniformly disperse the sepiolite in the water to obtain sepiolite dispersion liquid, and the dispersion liquid is kept stand for more than 72 hours without layering, so as to ensure the full dispersion and dissociation of nano sepiolite. In practical use, it is preferable to use alpha-sepiolite, and the concentration of the sepiolite dispersion is 1 to 10g/L.
(2) Mixing the sepiolite dispersion liquid and a bio-based acidic substance and then reacting to prepare sepiolite-based hybrid sol; preferably, the bio-based acidic substance in S2 is phytic acid or polyaspartic acid. In practical application, other acidic substances containing phosphorus and nitrogen can be used as biological base acidic substances.
In practical application, preferably, the concentration of the phytic acid solution is 5-15 g/L, and the concentration of the polyaspartic acid solution is 3-10 g/L. Preferably, the weight ratio of the sepiolite dispersion to the bio-based acidic substance is 0.2 to 1. Preferably, the sepiolite-based hybrid sol prepared in the step S2 is prepared at a temperature of 25-95 ℃ for 2-24 hours.
The skeleton structure of the alpha-sepiolite is shown in figure 1, and the alpha-sepiolite material is a fibrous flexible mineral in a 2:1 layer chain transition state, which consists of silicon oxygen tetrahedron and magnesium oxygen octahedron. When an acidic substance is added into sepiolite dispersion liquid, free hydrogen ions can be replaced with Mg atoms in a sepiolite skeleton structure to destroy the sepiolite three-dimensional skeleton structure and convert the sepiolite three-dimensional skeleton structure into an amorphous silica sol substance, and a large amount of Si-OH exists in the sol structure and is easy to generate condensation or generate chemical reaction with other substances with functional groups to generate new chemical bonds. In the invention, the sepiolite skeleton structure is converted from three-dimensional to amorphous by adopting the acidic substance, and meanwhile, the functional group in the acidic substance is subjected to covalent bond combination, hydrogen bond combination and the like with Si-OH in the sepiolite-based sol, so that the sol has better flame retardance.
(3) Coating the sepiolite-based hybrid sol on the surface of polyester-cotton fabric, and pre-drying at a certain temperature for 5-10 min, wherein the pre-drying temperature is 80-100 ℃ as a preferable choice; and baking after pre-baking, wherein the baking temperature is preferably 130-180 ℃ and the baking time is 2-10 min, so as to obtain the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric. In practical application, the weight gain rate of the coating can be 10% -100%, and the hybrid sol is coated on the surface of the polyester-cotton fabric and is mainly used for verifying the flame-retardant protection effect of the hybrid sol on the polyester-cotton fabric.
Example 1
The embodiment provides a preparation method of a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid, a phytic acid solution with the concentration of 15g/L and polyaspartic acid with the concentration of 5g/L according to the mass ratio of 5.6:12:6, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol, wherein the sepiolite-based hybrid sol has flame retardance;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) And pre-baking the polyester cotton fabric coated with the sepiolite-based hybrid sol at 90 ℃ for 5min, and then baking the polyester cotton fabric at 175 ℃ for 3min to obtain a flame-retardant type sepiolite-based hybrid sol coated polyester cotton fabric sample A.
In this example, sample a was prepared, and the fiber surface was uniformly coated with a layer of sepiolite-based hybrid sol film (organic/inorganic hybrid sol film) comprising the following components: the method comprises the steps of forming carboxyl groups in polyaspartic acid, phytic acid and sepiolite in the process of forming ester bonds with Si-OH on the surface of the sepiolite, carrying out structural modification on sepiolite-based hybrid sol, accessing a certain amount of polyaspartic acid structures, forming phosphate bonds with Si-OH in the sepiolite structures by phosphonic acid groups in the phytic acid, and accessing a phytic acid structure in the sepiolite-based hybrid sol. The organic/inorganic hybrid sol structure has a large number of-NH-, C= O, P-OH, P= O, si-OH groups and the like, and can form hydrogen bonds with-OH on the surface of cotton fibers, wherein phosphonic acid can form ester bond combination with-OH on the surface of cotton fibers in the baking process, so that the coating fastness of the hybrid sol film is improved. The hybrid sol has better compactness and elasticity, and can endow the polyester-cotton fabric with better flame retardance and mechanical strength.
Example 2
The embodiment provides a preparation method of a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid, a phytic acid solution with the concentration of 15g/L and polyaspartic acid with the concentration of 5g/L according to the mass ratio of 4:10:4, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol, wherein the sepiolite-based hybrid sol has flame retardance;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) And pre-baking the polyester cotton fabric coated with the sepiolite-based hybrid sol at 90 ℃ for 6min, and then baking the polyester cotton fabric at 170 ℃ for 3min to obtain a flame-retardant type sepiolite-based hybrid sol coated polyester cotton fabric sample B.
The sample B prepared in the embodiment is prepared by uniformly coating a sepiolite-based hybrid sol film (organic/inorganic hybrid sol film) on the surface of the fiber, wherein the sepiolite-based silica sol is mainly modified by polyaspartic acid and phytic acid; the carboxylic acid group and the phosphonic acid group in the sol can form ester bonds with C-OH on the surface of the polyester cotton fabric, NH-, C=O and P=O can form hydrogen bonds with the C-OH on the surface of the polyester cotton fabric, and the two acting forces can improve the coating fastness of the hybrid sol on the surface of the polyester cotton fabric. Sample B achieves V0 level flame retardance of flame retardant standard UL94, the flame-retardant time is 3s, the smoldering time is 10s, and the LOI is 29%; the breaking strength in the warp direction and the breaking elongation in the weft direction are 1147N and 380N respectively, and the breaking elongation in the warp direction and the breaking elongation in the weft direction are 17% and 15% respectively.
Example 3
The embodiment provides a preparation method of a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid, a phytic acid solution with the concentration of 15g/L and polyaspartic acid with the concentration of 5g/L according to the mass ratio of 5.6:14:4, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol, wherein the sepiolite-based hybrid sol has flame retardance;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) And pre-baking the polyester cotton fabric coated with the sepiolite-based hybrid sol at 90 ℃ for 6min, and then baking the polyester cotton fabric at 175 ℃ for 3min to obtain a flame-retardant type sepiolite-based hybrid sol coated polyester cotton fabric sample C.
The sample C prepared in this example was a fiber surface uniformly coated with a layer of sepiolite-based hybrid sol film (organic/inorganic hybrid sol film). Sample C achieves V0 level flame retardance of flame retardant standard UL94, the flame-retardant time is 10s, the smoldering time is 5s, and the LOI is 31%; the breaking strength in the warp direction and the breaking strength in the weft direction are 1008N and 366N respectively, and the breaking elongation in the warp direction and the breaking elongation in the weft direction are 18% and 17% respectively.
Example 4
The embodiment provides a preparation method of a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid, a phytic acid solution with the concentration of 15g/L and polyaspartic acid with the concentration of 5g/L according to the mass ratio of 4:14:6, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol, wherein the sepiolite-based hybrid sol has flame retardance;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) And pre-baking the polyester cotton fabric coated with the sepiolite-based hybrid sol at 90 ℃ for 6min, and then baking the polyester cotton fabric at 180 ℃ for 3min to obtain a flame-retardant type sepiolite-based hybrid sol coated polyester cotton fabric sample D.
In the sample D prepared in this example, the surface of the fiber is uniformly coated with a layer of sepiolite-based hybrid sol film (organic/inorganic hybrid sol film). Sample D achieves V0 grade flame retardance of flame retardance standard UL94, the flame-retardant time is 15s, the smoldering time is 7s, and the LOI is 31%; the breaking strength in the warp direction and the breaking elongation in the weft direction are 988N and 356N respectively, and the breaking elongation in the warp direction and the breaking elongation in the weft direction are 17% and 14% respectively.
Example 5
The embodiment provides a preparation method of a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid, a phytic acid solution with the concentration of 15g/L and polyaspartic acid with the concentration of 5g/L according to the mass ratio of 4:12:8, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol, wherein the sepiolite-based hybrid sol has flame retardance;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) And pre-baking the polyester cotton fabric coated with the sepiolite-based hybrid sol for 9min at 80 ℃, and then baking the polyester cotton fabric for 5min at 170 ℃ to obtain a flame-retardant type sepiolite-based hybrid sol coated polyester cotton fabric sample E.
In the sample E prepared in this example, the surface of the fiber is uniformly coated with a layer of sepiolite-based hybrid sol film (organic/inorganic hybrid sol film). Sample E achieves V0 level flame retardance of flame retardant standard UL94, the flame-retardant time is 15s, the smoldering time is 10s, and the LOI is 30%; the breaking strength in the warp direction and the breaking elongation in the weft direction are 1059N and 360N respectively, and the breaking elongation in the warp direction and the breaking elongation in the weft direction are 12% and 14% respectively.
Example 6
The embodiment provides a preparation method of a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid, a phytic acid solution with the concentration of 15g/L and polyaspartic acid with the concentration of 5g/L according to the mass ratio of 4.8:10:6, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol, wherein the sepiolite-based hybrid sol has flame retardance;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) And pre-baking the polyester cotton fabric coated with the sepiolite-based hybrid sol for 9min at 95 ℃, and then baking the polyester cotton fabric for 8min at 175 ℃ to obtain a flame-retardant type sepiolite-based hybrid sol coated polyester cotton fabric sample F.
In the sample F prepared in this example, the surface of the fiber is uniformly coated with a layer of sepiolite-based hybrid sol film (organic/inorganic hybrid sol film). Sample F achieves V0 level flame retardance of flame retardance standard UL94, the after-burning time is 17s, the smoldering time is 7s, and the LOI is 30%; the breaking strength in the warp direction and the breaking elongation in the weft direction are 941N and 363N respectively, and the breaking elongation in the warp direction and the breaking elongation in the weft direction are 13% and 14% respectively.
Example 7
The embodiment provides a preparation method of a flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid, a phytic acid solution with the concentration of 15g/L and polyaspartic acid with the concentration of 5g/L according to the mass ratio of 5.6:10:8, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol, wherein the sepiolite-based hybrid sol has flame retardance;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) And pre-baking the polyester cotton fabric coated with the sepiolite-based hybrid sol for 9min at 90 ℃, and then baking the polyester cotton fabric for 5min at 180 ℃ to obtain a flame-retardant type sepiolite-based hybrid sol coated polyester cotton fabric sample G.
In the sample G prepared in this example, the surface of the fiber is uniformly coated with a layer of sepiolite-based hybrid sol film (organic/inorganic hybrid sol film). Sample G achieves V0 level flame retardance of flame retardance standard UL94, the flame-continuing time is 0s, the smoldering time is 3s, and the LOI is 28%; the breaking strength in the warp direction and the weft direction are 1220N and 385N respectively, and the breaking elongation in the warp direction and the weft direction are 20% and 17% respectively.
Comparative example 1
The comparative example provides a preparation method of a flame retardant sepiolite-based hybrid sol coated polyester-cotton fabric only modified by phytic acid, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid and a phytic acid solution with the concentration of 15g/L according to the mass ratio of 5.6:12, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) And pre-baking the polyester cotton fabric coated with the sepiolite-based hybrid sol at 90 ℃ for 5min, and then baking the polyester cotton fabric at 175 ℃ for 3min to obtain a sepiolite-based hybrid sol coated polyester cotton fabric sample H.
The pure polyester cotton is marked as a sample CK, the flame-retardant sepiolite-based hybrid sol coated polyester cotton fabric prepared in the example 1 is marked as a sample A, and the product prepared in the comparative example 1 is marked as a sample H; in order to verify the washing fastness of the product, the sample A and the sample H are subjected to soaping and drying by referring to national standard GB/T3921.1-1997 textile color fastness experiment, and then the sample A-1 and the sample H-1 are respectively obtained.
Samples CK, A, H, A-1 and H-1 were analyzed for flame retardant properties using a vertical burn tester (YBG, ningbo textile Instrument Co., ltd.) and the data are shown in Table 1, and the photographs of the samples after testing are shown in FIG. 2.
The cotton fabric was subjected to oxygen limiting index test using a limiting oxygen index tester (LOI, 5801A-01, yang Yiwo, suzhou Kogyo Co., ltd.) and the data are shown in Table 1; the tensile properties of the cotton fabrics were tested using an electronic universal tester (WDW-50, shanghai Songton instruments Co., ltd.) and the data are shown in Table 2.
Table 1 sample flame retardant test data
Table 2 sample mechanical properties test data
As can be seen from the flame-retardant test data of the samples in Table 1, the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric (sample A) prepared by the invention has the advantages of greatly reduced continuous burning time and smoldering time, 11-72% rise of limiting oxygen index, and reduced burning carbon length of the polyester-cotton fabric after flame-retardant treatment, and self-extinguishing property as can be seen from FIG. 2. The data show that the flame retardant property of the polyester-cotton fabric is greatly improved after flame retardant treatment, and the polyester-cotton fabric still has a certain flame retardance after water washing.
According to fig. 2, the hybrid sol can impart a certain flame retardancy to the polyester-cotton fabric. After the sepiolite-based hybrid sol was coated on the polyester cotton fabric, the pure polyester cotton sample CK (fig. 2 (a)) was all converted into carbon after the vertical burning test, and the damaged length after burning of the sepiolite-based hybrid sol coated polyester cotton fabric sample a (fig. 2 (e)) was less than 2cm. As shown in fig. 3, the polyester cotton fabrics before and after the standard water washing were found to have a higher amount of char residue than the uncoated pure polyester cotton (sample CK) even with the standard water washed flame retardant sepiolite-based hybrid sol coated polyester cotton material (sample a-1).
In summary, the flame retardant finishing process of the invention can impart better durable flame retardance to polyester-cotton fabrics. From the mechanical property data of the materials in Table 2, it can be concluded that the prepared flame-retardant sepiolite-based hybrid sol coated polyester-cotton fabric has better mechanical property, and the flame-retardant finishing method in the invention is better and is more suitable for large-scale application of the polyester-cotton fabric.
Comparative example 2
The comparative example provides a preparation method of an aspartic acid modified flame retardant sepiolite-based hybrid sol coated polyester-cotton fabric, which comprises the following steps:
(1) Dispersing sepiolite in water, and uniformly stirring by using a homogenizer to obtain sepiolite dispersion liquid with the concentration of 6 g/L;
(2) Mixing the sepiolite dispersion liquid and aspartic acid solution with the concentration of 5g/L according to the mass ratio of 5.6:6, mixing, and reacting for 2 hours at 90 ℃ to obtain sepiolite-based hybrid sol;
(3) Coating the sepiolite-based hybrid sol on polyester cotton fabric, and controlling the weight gain rate of the coating to be 25%;
(4) The polyester cotton fabric coated with the sepiolite-based hybrid sol is pre-baked for 5min at 90 ℃ and then baked for 3min at 175 ℃ to obtain a sepiolite-based hybrid sol coated polyester cotton fabric sample M.
The final prepared sample M has a post-ignition time of 15s, a smoldering time of 10s and an LOI of 26%; the breaking strength in the warp direction and the breaking elongation in the weft direction are respectively 1020N and 370N, and the breaking elongation in the warp direction and the breaking elongation in the weft direction are respectively 14% and 16%.
Compared with the sample A prepared in the example 1, the after-burning time and smoldering burning time of the sample M are longer than those of the sample A, the breaking strength in the warp direction and the weft direction is smaller than that of the sample A, and the breaking elongation in the warp direction and the weft direction is smaller than that of the sample A, because the polyester cotton fabric in the sample M is coated by the aspartic acid solution hybridization sol, and the flame retardant property is inferior to that of the polyester cotton fabric coated by the phytic acid and aspartic acid hybridization sol in the example 1, so that the after-burning time and the smoldering burning time are longer, and the flame retardant property is poorer.
The main components of the coating sol in the sample M are sea bubble silica sol and polyaspartic acid, wherein the polyaspartic acid structure contains an-NH-group and has certain flame retardance, and the coating sol has certain catalytic carbonization performance on polyester cotton fabric under the high temperature condition; the hybrid sol in the sample A contains polyaspartic acid and phytic acid, the substance structures respectively contain N, P elements, and the polyaspartic acid and the phytic acid have a certain synergistic flame-retardant effect, so that the hybrid sol in the sample A is coated on the surface of the polyester-cotton fabric, and the polyester-cotton fabric has better carbon forming promotion property.
The sepiolite-based hybrid sol prepared by the method overcomes the defects of small molecular weight and large brittleness of the traditional silica sol prepared by taking silicate as a raw material, has a certain molecular network structure, can form a film with certain flexibility on the surface of a textile, and endows the textile material with flame retardance and certain mechanical property.
The above embodiment is only a preferred embodiment of the present invention, but it is not intended to limit the present invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, all the technical schemes obtained by adopting the equivalent substitution or equivalent transformation are within the protection scope of the invention.
Claims (10)
1. The preparation method of the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric is characterized by comprising the following specific steps of:
s1: dispersing sepiolite in water, and stirring to obtain sepiolite dispersion liquid;
s2: mixing the sepiolite dispersion liquid and the bio-based acidic substance and then reacting to prepare sepiolite-based hybrid sol;
s3: and coating the sepiolite-based hybrid sol on the surface of the polyester cotton fabric, and baking after pre-baking to obtain the flame-retardant sepiolite-based hybrid sol coated polyester cotton fabric.
2. The method for preparing the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric according to claim 1, wherein the sepiolite is alpha-sepiolite.
3. The method for preparing the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric according to claim 1, wherein the concentration of the sepiolite dispersion liquid is 1-10 g/L, and the sepiolite-based hybrid sol-coated polyester-cotton fabric is obtained by stirring by a homogenizer.
4. The method for preparing the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric according to claim 1, wherein the bio-based acidic substance adopts phytic acid and polyaspartic acid.
5. The method for preparing the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric according to claim 4, wherein the concentration of the phytic acid solution is 5-15 g/L; the concentration of the polyaspartic acid solution is 3-10 g/L.
6. The method for preparing the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric according to claim 1, wherein the weight ratio of the sepiolite dispersion liquid to the bio-based acidic substance is 0.2-1.
7. The method for preparing the flame-retardant sepiolite-based hybrid sol coated polyester-cotton fabric according to claim 1, wherein the temperature in the preparation of the sepiolite-based hybrid sol is 25-95 ℃ and the time is 2-24 h.
8. The method for preparing the flame retardant sepiolite-based hybrid sol coated polyester-cotton fabric according to claim 1, wherein the weight gain rate of the coating is 10% -100%.
9. The method for preparing the flame-retardant sepiolite-based hybrid sol-coated polyester-cotton fabric according to claim 1, wherein the pre-baking temperature is 80-100 ℃ and the pre-baking time is 5-10 min; the baking temperature is 130-180 ℃ and the baking time is 2-10 min.
10. A polyester-cotton fabric coated with a flame retardant sepiolite-based hybrid sol according to any one of claims 1 to 9.
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