CN117385638A - Flame-retardant silk fabric and preparation method and application thereof - Google Patents
Flame-retardant silk fabric and preparation method and application thereof Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 116
- 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 115
- 239000004744 fabric Substances 0.000 title claims abstract description 102
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title description 3
- BYSUYBCCLCSGPR-UHFFFAOYSA-N 1h-pyrazol-5-yloxyboronic acid Chemical compound OB(O)OC1=CC=NN1 BYSUYBCCLCSGPR-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000007788 liquid Substances 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 230000010355 oscillation Effects 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 15
- 239000007789 gas Substances 0.000 abstract description 13
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 abstract description 10
- 239000001301 oxygen Substances 0.000 abstract description 10
- 238000002485 combustion reaction Methods 0.000 abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 6
- 230000002411 adverse Effects 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 abstract description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical group OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005187 foaming Methods 0.000 abstract description 3
- 239000004088 foaming agent Substances 0.000 abstract description 3
- 230000004927 fusion Effects 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract description 3
- 238000002955 isolation Methods 0.000 abstract description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 238000009988 textile finishing Methods 0.000 abstract description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract 1
- 229910052796 boron Inorganic materials 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- 150000001875 compounds Chemical class 0.000 description 7
- 239000000835 fiber Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- LMBFAGIMSUYTBN-MPZNNTNKSA-N teixobactin Chemical compound C([C@H](C(=O)N[C@@H]([C@@H](C)CC)C(=O)N[C@@H](CO)C(=O)N[C@H](CCC(N)=O)C(=O)N[C@H]([C@@H](C)CC)C(=O)N[C@@H]([C@@H](C)CC)C(=O)N[C@@H](CO)C(=O)N[C@H]1C(N[C@@H](C)C(=O)N[C@@H](C[C@@H]2NC(=N)NC2)C(=O)N[C@H](C(=O)O[C@H]1C)[C@@H](C)CC)=O)NC)C1=CC=CC=C1 LMBFAGIMSUYTBN-MPZNNTNKSA-N 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- TZHYBRCGYCPGBQ-UHFFFAOYSA-N [B].[N] Chemical compound [B].[N] TZHYBRCGYCPGBQ-UHFFFAOYSA-N 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XWSGEVNYFYKXCP-UHFFFAOYSA-N 2-[carboxymethyl(methyl)amino]acetic acid Chemical compound OC(=O)CN(C)CC(O)=O XWSGEVNYFYKXCP-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000002351 wastewater Substances 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a flame-retardant silk fabric and a preparation method and application thereof, and belongs to the technical field of textile finishing. According to the invention, pyrazolyl borate is used as a flame retardant, wherein the borate structure can form a glassy fusion covering in the combustion process, so that the stability of a carbon layer is improved, the flame retardant effect is achieved, and further, nitrogen-containing components in the flame retardant can generate ammonia, nitrogen and other flame-retardant gases in the combustion process, so that the concentration of the combustible gases can be diluted, and the flame-retardant can be used as a foaming agent of a carbon layer to form a foaming expansion type porous carbon layer, so that the combustible gases are prevented from entering a gas phase to achieve the effects of heat insulation and oxygen isolation; the synergistic effect of boron and nitrogen can effectively improve the flame retardant property of silk, and can improve the mechanical property of silk fabric without adverse effect on softness and smoothness.
Description
Technical Field
The invention relates to the technical field of textile finishing, in particular to a flame-retardant silk fabric and a preparation method and application thereof.
Background
Silk belongs to natural protein fibers, has the advantages of elegant luster, comfortable wearing, good hygroscopicity, moisture permeability, softness and the like, and has wide application in clothing, curtains, bedding and the like. However, silk fabrics have a limiting oxygen index of about 23%, are flammable, and can produce a large amount of toxic substances such as CO and HCN during combustion. Therefore, compared with silk fabrics, the flame-retardant finishing is performed, so that the silk fabrics are beneficial to expanding the application of the silk fabrics, and have important significance for protecting the life and property safety of people.
The prior art uses halogen flame retardant to improve the flame retardant property of silk, but the halogen flame retardant releases toxic and corrosive hydrogen halide gas in the combustion process, so that the halogen flame retardant seriously pollutes the environment and endangers human health. Along with the enhancement of environmental awareness, the research of the flame retardant is gradually developed towards the green, environment-friendly and efficient directions. The halogen-free phosphorus flame retardant is paid more attention, but the problems of large flame retardant use amount, poor physical properties of the finished silk fabric and the like exist, and a large amount of phosphorus-containing wastewater is generated to influence ecological environment when the phosphorus flame retardant is used in production.
Therefore, how to improve the flame retardant property of silk fabric and ensure the physical property of silk fabric becomes a difficult problem in the prior art.
Disclosure of Invention
The invention aims to provide a flame-retardant silk fabric, and a preparation method and application thereof. The silk fabric prepared by the preparation method provided by the invention has excellent flame retardant property, and meanwhile, the mechanical strength of the silk fabric can be improved, and the softness and smoothness of the silk fabric are maintained.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a flame-retardant silk fabric, which comprises the following steps:
(1) Mixing pyrazolyl borate and a solvent to obtain flame-retardant finishing liquid;
the structure of the pyrazolyl borate is shown as a formula I or a formula II:
(2) And (3) oscillating the silk fabric in the flame-retardant finishing liquid obtained in the step (1) to obtain the flame-retardant silk fabric.
Preferably, the solvent in the step (1) is a mixed solution of ethanol and water.
Preferably, the volume ratio of the ethanol to the water is 1: (2.5-4).
Preferably, the concentration of the pyrazolyl borate in the flame retardant finishing liquid in the step (1) is 0.05-0.25 mol/L.
Preferably, the mass ratio of the pyrazolyl borate in the silk fabric and the flame retardant finishing liquid in the step (2) is 1: (0.6-4.5).
Preferably, the temperature of the oscillation in the step (2) is 40-80 ℃, and the time of the oscillation is 2-12 h.
Preferably, the step (2) further comprises water washing and drying after the oscillating is completed.
Preferably, the drying temperature is 40-80 ℃ and the drying time is 2-10 h.
The invention provides the flame-retardant silk fabric prepared by the preparation method.
The invention also provides application of the flame-retardant silk fabric in clothing, curtains and bedding.
The invention provides a preparation method of a flame-retardant silk fabric, which comprises the following steps: (1) Mixing pyrazolyl borate and a solvent to obtain flame-retardant finishing liquid; the structure of the pyrazolyl borate is shown as a formula I or a formula II:
(2) And (3) oscillating the silk fabric in the flame-retardant finishing liquid obtained in the step (1) to obtain the flame-retardant silk fabric. According to the invention, pyrazolyl borate is used as a flame retardant, wherein the borate structure can form a glassy fusion covering in the combustion process, so that the stability of a carbon layer is improved, the flame retardant effect is achieved, and further, nitrogen-containing components in the flame retardant can generate ammonia, nitrogen and other flame-retardant gases in the combustion process, so that the concentration of the combustible gases can be diluted, and the flame-retardant can be used as a foaming agent of a carbon layer to form a foaming expansion type porous carbon layer, so that the combustible gases are prevented from entering a gas phase to achieve the effects of heat insulation and oxygen isolation; the boron-nitrogen synergistic effect enables the compound of the formula II to effectively improve the flame retardant property of silk, and simultaneously can improve the mechanical property of silk fabric without adversely affecting the softness and smoothness of the silk fabric. The results of the examples show that the limiting oxygen index of the flame-retardant silk fabric prepared by the preparation method is above 25.8%, the flame-retardant silk fabric belongs to a flame-retardant product, the mechanical strength of the silk fabric is improved, and the softness and smoothness of the silk fabric are basically unchanged.
Drawings
FIG. 1 is an infrared spectrum of a compound of formula I, a compound of formula II, a flame retardant silk fabric of examples 1-2 and a silk fabric of comparative example 1 according to the present invention;
FIG. 2 is an SEM image of carbon residue after vertical burning of the silk fabric of comparative example 1 of the present invention;
FIG. 3 is an SEM image of carbon residue after vertical burning of the flame retardant silk fabric of example 1 of the present invention;
FIG. 4 is an SEM image of carbon residue after vertical burning of the flame retardant silk fabric of example 2 of the present invention;
fig. 5 is a stress-strain graph of the flame retardant silk fabrics of examples 1-2 and the silk fabric of comparative example 1 according to the present invention.
Detailed Description
The invention provides a preparation method of a flame-retardant silk fabric, which comprises the following steps:
(1) Mixing pyrazolyl borate and a solvent to obtain flame-retardant finishing liquid;
the structure of the pyrazolyl borate is shown as a formula I or a formula II:
(2) And (3) oscillating the silk fabric in the flame-retardant finishing liquid obtained in the step (1) to obtain the flame-retardant silk fabric.
The source of each raw material is not particularly limited unless specifically stated, and commercially available products known to those skilled in the art may be used. In embodiments of the invention, the compound of formula i is preferably purchased at An Naiji; the compounds of the formula II are preferably synthesized according to the procedure described in the literature [ Organic Letters,2020,22 (24): 9408-9414 ], in particular: 12.6g of 1-methyl-1H-pyrazole-4-boric acid, 17.6g of N-methyliminodiacetic acid, 60mL of toluene and 30mL of dimethyl sulfoxide are added into a 250mL reaction bottle, heated and refluxed for 6 hours, cooled to room temperature after the reaction is finished, distilled under reduced pressure to remove the solvent to obtain an oily mixture, and recrystallized with water to obtain 12.3g of a white solid, namely a compound of formula II, wherein the specific reaction equation is as follows:
according to the invention, the pyrazolyl borate and the solvent are mixed to obtain the flame-retardant finishing liquid.
In the invention, the structure of the pyrazolyl borate is shown as a formula I or a formula II:
in the invention, the pyrazolyl borate is used as a flame retardant, wherein the borate structure can form a glassy fusion covering in the combustion process, so that the stability of a carbon layer is improved, the flame retardant effect is achieved, and further, nitrogen-containing components in the flame retardant can generate flame-retardant gases such as ammonia, nitrogen and the like in the combustion process, so that the concentration of the combustible gases can be diluted, and the flame-retardant can be used as a foaming agent of a carbon layer to form a foaming expansion porous carbon layer, so that the combustible gases are prevented from entering a gas phase to achieve the effects of heat insulation and oxygen isolation; the boron-nitrogen synergistic effect effectively improves the flame retardant property of silk, can improve the mechanical property of silk fabric, does not adversely affect the softness and smoothness of the silk fabric, and compared with halogen-series and phosphorus-series flame retardants, the flame retardant disclosed by the invention has lower toxicity and is more environment-friendly.
In the present invention, the solvent is preferably a mixed solution of ethanol and water; the volume ratio of the ethanol to the water is preferably 1: (2.5 to 4), more preferably 1: (2.5-3). The invention limits the composition of the solvent and the dosage of each component in the above range, so that the flame retardant can be better adsorbed by silk.
In the present invention, the concentration of the pyrazolyl borate in the flame retardant finishing liquid is preferably 0.05 to 0.25mol/L, more preferably 0.15 to 0.25mol/L. The concentration of the pyrazolyl borate in the flame-retardant finishing liquid is limited in the range, so that the pyrazolyl borate can be more fully dissolved.
The operation of mixing the pyrazolyl borate and the solvent is not particularly limited, and the material mixing technical scheme well known to the person skilled in the art can be adopted.
After the flame-retardant finishing liquid is obtained, the silk fabric is oscillated in the flame-retardant finishing liquid to obtain the flame-retardant silk fabric.
In the present invention, the silk fabric is preferably a crepe satin silk fabric.
In the invention, the mass ratio of the pyrazolyl borate in the silk fabric and the flame retardant finishing liquid is preferably 1: (0.6 to 4.5), more preferably 1: (1.0 to 4.5), more preferably 1: (2.0-4.5). According to the invention, the mass ratio of the pyrazolyl borate in the silk fabric and the flame-retardant finishing liquid is limited in the range, so that the silk fabric can adsorb more pyrazolyl borate flame retardant, the flame retardant property and the mechanical property of the silk fabric are further improved, and the softness and the smoothness of the silk fabric are not adversely affected.
In the present invention, the temperature of the oscillation is preferably 40 to 80 ℃, more preferably 50 to 60 ℃; the time of the oscillation is preferably 2 to 12 hours, more preferably 6 to 7 hours; the frequency of the oscillation is preferably 150RPM. The invention limits the temperature and time of oscillation within the above range, so that silk fabric can absorb more pyrazolyl borate flame retardant.
After the oscillation is completed, the fabric after the oscillation is preferably washed with water and dried sequentially.
The operation of the water washing is not particularly limited, and the flame-retardant finishing liquid is cleaned by adopting a water washing technical scheme which is well known to a person skilled in the art.
In the present invention, the drying temperature is preferably 40 to 80 ℃, more preferably 60 to 70 ℃; the drying time is preferably 2 to 10 hours, more preferably 3 to 4 hours.
According to the invention, the pyrazolyl borate is used as the flame retardant, so that the flame retardant property of silk is improved, the mechanical property of silk is improved, and meanwhile, the softness and smoothness of silk are not influenced.
The invention provides the flame-retardant silk fabric obtained by the preparation method.
The flame-retardant silk fabric prepared by the invention has excellent flame retardant property, mechanical property, softness and smoothness.
The invention also provides application of the flame-retardant silk fabric in clothing, curtains and bedding.
The operation of the application of the flame-retardant silk fabric in clothing, curtains and bedding is not particularly limited, and the technical scheme of the application of the flame-retardant silk fabric in clothing, curtains and bedding, which is well known to those skilled in the art, is adopted.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) 2.9630g of pyrazolyl borate is dissolved in 50mL of mixed solution of ethanol and water, the volume ratio of the ethanol to the water is 1:2.5, and the flame-retardant finishing liquid is obtained, wherein the concentration of the pyrazolyl borate in the flame-retardant finishing liquid is 0.25mol/L; the structure of the pyrazolyl borate is shown as a formula II:
(2) Immersing the plain crepe satin silk fabric (8.9 multiplied by 30 cm) into the flame-retardant finishing liquid (the mass ratio of the silk fabric to the pyrazolyl borate in the flame-retardant finishing liquid is 1:4.4), oscillating at a constant temperature of 50 ℃ for 7 hours (the oscillating frequency is 150 RPM), taking out the silk fabric, washing with water for three times, and drying at 60 ℃ for 3 hours to obtain the flame-retardant silk fabric.
Example 2
(1) 2.601g of pyrazolyl borate is dissolved in 50mL of mixed solution of ethanol and water, the volume ratio of the ethanol to the water is 1:2.5, and the flame-retardant finishing liquid is obtained, wherein the concentration of the pyrazolyl borate in the flame-retardant finishing liquid is 0.25mol/L; the structure of the pyrazolyl borate is shown as a formula I:
(2) Immersing the plain crepe satin silk fabric (8.9 multiplied by 30 cm) into the flame-retardant finishing liquid (the mass ratio of the silk fabric to the pyrazolyl borate in the flame-retardant finishing liquid is 1:3.9), oscillating at a constant temperature of 50 ℃ for 7 hours (the oscillating frequency is 150 RPM), taking out the silk fabric, washing with water for three times, and drying at 60 ℃ for 3 hours to obtain the flame-retardant silk fabric.
Example 3
The amount of the pyrazolyl borate in the flame retardant finishing liquid in example 1 was replaced with 0.5926g, at this time, the concentration of the pyrazolyl borate in the flame retardant finishing liquid was 0.05mol/L, the mass ratio of the pyrazolyl borate in the silk fabric to the flame retardant finishing liquid was 1:0.9, and other parameters were the same as those in example 1.
Example 4
The amount of the pyrazolyl borate in example 1 was replaced with 1.7778g, at this time, the concentration of the pyrazolyl borate in the flame retardant finishing liquid was 0.15mol/L, the mass ratio of the silk fabric to the pyrazolyl borate in the flame retardant finishing liquid was 1:2.7, and other parameters were the same as those in example 1.
Comparative example 1
Untreated crepe satin silk fabric.
The limiting oxygen index LOI of the silk fabrics of examples 1 to 4 and comparative example 1 were tested according to GB/T5455-2014 Experimental oxygen index method for Combustion Performance of textiles, and the results are shown in Table 1.
TABLE 1 limiting oxygen index of silk fabrics of examples 1-4 and comparative example 1
| LOI/％ | |
| Comparative example 1 | 24.2 |
| Example 1 | 28.3 |
| Example 2 | 27.5 |
| Example 3 | 25.8 |
| Example 4 | 26.1 |
As can be seen from Table 1, after the flame retardant is used for treating the silk fabric, the limiting oxygen index of the silk fabric is improved from 24.2% to more than 25.8%, and the maximum oxygen index of the silk fabric can be up to 28.3%, so that the silk fabric belongs to a flame-retardant product, the flame retardant property of the silk fabric is improved, and meanwhile, compared with the compound of the formula I, the flame retardant property of the silk fabric treated by the compound of the formula II is better.
Infrared ray of compound of formula I, compound of formula II, flame retardant silk fabrics of examples 1-2 and silk fabric of comparative example 1The spectrum is shown in FIG. 1. As can be seen from FIG. 1, the infrared spectra of example 1 and example 2 were obtained at 1384cm -1 An absorption peak, which is a stretching vibration peak of B-O bond, appears in the vicinity, example 2 at 1742cm -1 An absorption peak of c=o appears nearby, and 1233cm -1 The absorption of the characteristic peak of the C-N bond at the position is enhanced, which indicates that the flame retardant is smoothly grafted on the silk fabric.
SEM images of carbon residue after vertical burning of the silk fabrics of comparative example 1 and the flame retardant silk fabrics of examples 1 to 2 are shown in fig. 2 to 4, respectively. As can be seen from fig. 2 to 4, the coke residue surface of the silk fabric is broken and incomplete, and the complete holes with thin films appear on the surfaces of the carbon layers of example 1 and example 2, so that a typical expansion barrier carbon layer is formed, and the silk fabric can be protected from further burning.
The stress-strain curves of the flame retardant silk fabrics of examples 1 to 2 and the silk fabric of comparative example 1 are shown in fig. 5, and the data of tensile stress and elongation at break thereof are shown in table 2.
TABLE 2 tensile stress and elongation at break of silk fabrics of examples 1-2 and comparative example 1
| Sample preparation | Tensile stress (cN) | Elongation at break (%) |
| Comparative example 1 | 86.8±0.63 | 26.78±1.89 |
| Example 1 | 100.29±6.87 | 28.09±1.75 |
| Example 2 | 109.81±5.55 | 30.49±2.85 |
As can be seen from fig. 5 and table 2, the untreated silk fiber of comparative example 1 has a tensile strength of 86.80cN and an elongation at break of 26.78%, and the mechanical strength of the silk fiber is significantly enhanced after the introduction of the pyrazolyl borate, compared with the untreated silk fiber, and the elongation at break of examples 1 and 2 are 28.09% and 30.49%, respectively, and the tensile strength is improved by 15.54% and 26.51%, respectively, indicating that the pyrazolyl borate is effective in improving the mechanical strength of silk.
The softness and smoothness of the flame retardant silk fabrics of examples 1-2 and the silk fabric of comparative example 1 were tested and the results are shown in table 3.
Table 3 softness and smoothness of the flame retardant silk fabrics of examples 1-2 and the silk fabric of comparative example 1
| Sample preparation | Softness and softness | Smoothness degree |
| Comparative example 1 | 97.77±0.77 | 61.00±0.23 |
| Example 1 | 94.14±1.13 | 56.23±0.24 |
| Example 2 | 95.66±0.81 | 58.31±0.37 |
It can be seen from table 3 that the smoothness and softness of the silk fabric flame-retardant finished with pyrazolyl borate are not much different from those of the silk fabric not finished.
In conclusion, the silk fabric subjected to flame retardant finishing by the pyrazolyl borate has good flame retardant property and mechanical property, and has no influence on the smoothness and softness of the silk fabric basically.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the flame-retardant silk fabric comprises the following steps:
(1) Mixing pyrazolyl borate and a solvent to obtain flame-retardant finishing liquid;
the structure of the pyrazolyl borate is shown as a formula I or a formula II:
(2) And (3) oscillating the silk fabric in the flame-retardant finishing liquid obtained in the step (1) to obtain the flame-retardant silk fabric.
2. The method according to claim 1, wherein the solvent in the step (1) is a mixed solution of ethanol and water.
3. The method according to claim 2, wherein the volume ratio of ethanol to water is 1: (2.5-4).
4. The method according to claim 1, wherein the concentration of the pyrazolyl borate in the flame retardant finishing liquid in the step (1) is 0.05-0.25 mol/L.
5. The preparation method according to claim 1, wherein the mass ratio of the pyrazolyl borate in the silk fabric and the flame retardant finishing liquid in the step (2) is 1: (0.6-4.5).
6. The method according to claim 1, wherein the temperature of the oscillation in the step (2) is 40 to 80 ℃ and the time of the oscillation is 2 to 12 hours.
7. The method according to claim 1, wherein the step (2) further comprises washing with water and drying sequentially after the completion of the shaking.
8. The method according to claim 7, wherein the drying temperature is 40 to 80 ℃ and the drying time is 2 to 10 hours.
9. The flame retardant silk fabric prepared by the preparation method of any one of claims 1 to 8.
10. Use of the flame retardant silk fabric of claim 9 in clothing, curtains and bedding.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311616704.7A CN117385638A (en) | 2023-11-30 | 2023-11-30 | Flame-retardant silk fabric and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311616704.7A CN117385638A (en) | 2023-11-30 | 2023-11-30 | Flame-retardant silk fabric and preparation method and application thereof |
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