CN116289216A - Preparation method of halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric - Google Patents
Preparation method of halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric Download PDFInfo
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- CN116289216A CN116289216A CN202310517841.9A CN202310517841A CN116289216A CN 116289216 A CN116289216 A CN 116289216A CN 202310517841 A CN202310517841 A CN 202310517841A CN 116289216 A CN116289216 A CN 116289216A
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- 239000004744 fabric Substances 0.000 title claims abstract description 177
- 229920000728 polyester Polymers 0.000 title claims abstract description 152
- 239000003063 flame retardant Substances 0.000 title claims abstract description 107
- 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 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- RGHHSNMVTDWUBI-UHFFFAOYSA-N 4-hydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1 RGHHSNMVTDWUBI-UHFFFAOYSA-N 0.000 claims abstract description 112
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 71
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 70
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 70
- 239000000661 sodium alginate Substances 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000005406 washing Methods 0.000 claims abstract description 30
- 125000002091 cationic group Chemical group 0.000 claims abstract description 26
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001338 self-assembly Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- 238000001035 drying Methods 0.000 claims description 48
- 239000011259 mixed solution Substances 0.000 claims description 42
- 238000005096 rolling process Methods 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 230000004584 weight gain Effects 0.000 claims description 11
- 235000019786 weight gain Nutrition 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 229920000742 Cotton Polymers 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 229920001661 Chitosan Polymers 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 150000004676 glycans Polymers 0.000 description 6
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 150000004804 polysaccharides Polymers 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000002262 Schiff base Substances 0.000 description 2
- 150000004753 Schiff bases Chemical class 0.000 description 2
- 125000003172 aldehyde group Chemical group 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 239000000675 fabric finishing Substances 0.000 description 1
- 238000009962 finishing (textile) Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012876 topography 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
- 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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—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
- D06M13/152—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 having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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Abstract
The invention relates to a preparation method of halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric, which adopts a layer-by-layer self-assembly method to deposit cationic polyacrylamide, oxidized sodium alginate and parahydroxyben-zaldehyde on the surface of the polyester fabric to prepare the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric; the damage length of the prepared halogen-phosphorus-free flame-retardant anti-dripping polyester fabric is not more than 12.2cm, the dripping is 0 drop, absorbent cotton is not ignited, the carbon residue is not less than 28.5%, and the damage length after 15 times of water washing is not more than 14.3cm; the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is simple in preparation, and the char formation performance, flame-retardant anti-dripping performance and environmental friendliness of the polyester fabric are effectively improved.
Description
Technical Field
The invention belongs to the technical field of flame-retardant fabrics, and relates to a preparation method of a halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric.
Background
The polyester fiber is a synthetic fiber with highest yield, fastest development and the most extensive application range at present, and has the excellent characteristics of good wear resistance, stiffness, friction resistance, chemical corrosion resistance and the like. Therefore, polyester fibers are widely used in the fields of clothing, bedding, curtains, sofas, carpets and the like, however, the fields have high requirements on flame retardant properties of textiles. The polyester fiber belongs to inflammable fiber, can not self-extinguish after being ignited and generates molten drops, thus being easy to cause secondary fire. The development of the flame-retardant polyester fabric has important practical significance.
The demands of people on self life health, environmental protection and ecological sustainable development are increasing, and the use of traditional halogen flame retardants is gradually forbidden. The phosphorus element easily causes eutrophication of water, so that the use of phosphorus-containing flame retardants is gradually limited. The development of a halogen-free and phosphorus-free flame retardant system and the preparation of the efficient flame retardant anti-dripping polyester fabric are significant.
Document 1 (chitosan/sodium alginate coating and flame-retardant polyester fabric research [ J ]. Fire-fighting science and technology, 2020,39 (10): 1421-1424.) utilizes bio-based chitosan and sodium alginate to improve the flame-retardant property of polyester fabric by means of electrostatic layer-by-layer self-assembly technology. However, sodium alginate has low thermal stability, cannot form metal oxide with high thermal stability, has low nitrogen content of chitosan and more flammable polysaccharide groups, so that the flame retardant efficiency of a chitosan/sodium alginate system is poor, the flame retardant performance of the modified polyester fabric is poor, and the modified polyester fabric is completely combusted in a vertical combustion test and has molten drops.
The development of a halogen-free and phosphorus-free flame-retardant system for polyester fabrics is a hot spot and a difficult point in the field of flame-retardant textiles, so that a preparation method of the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabrics is researched to improve the char formation performance and the flame-retardant anti-dripping performance of the polyester fabrics, and the problem that the existing halogen-free and phosphorus-free flame-retardant system has poor flame-retardant anti-dripping performance on the polyester fabrics is solved, and the halogen-free and phosphorus-free flame-retardant system has very important significance.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric.
In order to achieve the above purpose, the invention adopts the following scheme:
the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric adopts a layer-by-layer self-assembly method to deposit cationic polyacrylamide, oxidized sodium alginate and parahydroxybenzaldehyde on the surface of the polyester fabric, so as to prepare the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric.
As a preferable technical scheme:
the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric comprises the following specific steps:
(1) Firstly, dissolving oxidized sodium alginate and parahydroxybenzaldehyde in a mixed solution of water and ethanol to obtain a mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, then soaking a polyester fabric in the mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, taking out, removing excessive water on the fabric by adopting a small padder, and sequentially carrying out drying and water washing treatment;
(2) Immersing the polyester fabric treated in the step (1) into cationic polyacrylamide aqueous solution, taking out, removing excessive water on the fabric by adopting a small padder, and sequentially carrying out drying and washing treatment;
in the step (1) and the step (2), the water washing treatment is helpful for removing unreacted oxidized sodium alginate, parahydroxyben-zaldehyde and cationic polyacrylamide on the surface, and is helpful for improving the uniformity and durability of the coating;
the method has the advantages that the p-hydroxybenzaldehyde and the cationic polyacrylamide can react in a covalent bond way, so that the mixed solution cannot be immersed, and if the cationic polyacrylamide, the oxidized sodium alginate and the p-hydroxybenzaldehyde are respectively immersed in the fabric independently, the steps are more and more complicated, so that the method adopts the mode of preparing the mixed solution by the oxidized sodium alginate and the p-hydroxybenzaldehyde, immersing the mixed solution first, and then immersing the cationic polyacrylamide solution to finish the polyester fabric;
(3) And (3) alternately repeating the step (1) and the step (2) for a plurality of times, and depositing oxidized sodium alginate, parahydroxybenzaldehyde and cationic polyacrylamide on the surface of the polyester fabric to prepare the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric.
According to the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric, the mass concentration of oxidized sodium alginate is 1-3% and the mass concentration of parahydroxyben-zaldehyde is 2-4% in the mixed solution of oxidized sodium alginate and parahydroxyben-zaldehyde; the high usage of oxidized sodium alginate is beneficial to depositing on the surface of the polyester fabric, but the too high usage leads to too thick solution, which is easy to lead to uneven coating on the surface of the polyester fabric; the dosage of the p-hydroxybenzaldehyde is high, which is helpful for improving the flame-retardant and anti-dripping performance of the polyester fabric, and the excessive use is wasteful.
According to the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric, the volume ratio of ethanol in the mixed solution of water and ethanol in the step (1) is 20-40%, and the addition of ethanol is beneficial to the dissolution of p-hydroxybenzaldehyde.
According to the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric, in the step (1), the rolling residual rate of the polyester fabric is 80-100%, the higher the rolling residual rate is, the higher the fabric liquid carrying amount and the flame retardant amount are, the better the flame-retardant effect is, but the unevenness is easily caused by the overhigh rolling residual rate; the drying temperature is 70-80 ℃, and the drying time is 5-10 min.
According to the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric, in the step (2), the mass concentration of the cationic polyacrylamide aqueous solution is 1-3%, the cationic polyacrylamide aqueous solution is high in concentration, deposition on the surface of the polyester fabric is facilitated, but the solution is too viscous due to the fact that the concentration is too high, and uneven coating on the surface of the polyester fabric is easily caused.
According to the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric, in the step (2), the rolling residual rate of the polyester fabric is 80-100%, the higher the rolling residual rate is, the higher the fabric liquid carrying amount and the flame retardant amount are, the better the flame-retardant effect is, but the unevenness is easily caused by the overhigh rolling residual rate; the drying temperature is 70-80 ℃, and the drying time is 5-10 min.
According to the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric, the number of times of alternating repetition in the step (3) is 3-7, and the weight gain rate of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 12.5-21.2% (the weight gain rate refers to the percentage of the quality difference before and after fabric finishing to the quality of the polyester fabric); the more the number of repeated operations, the more the amount of flame retardant deposited on the surface of the polyester fabric is, the more the flame retardant is facilitated, but the too high flame retardant is wasted, and in the provided range, the modified polyester fabric has better char formation performance and flame retardant anti-dripping performance.
According to the preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric, the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is subjected to a combustion performance test, the damage length of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is not more than 12.2cm, the dripping is 0 drop, absorbent cotton is not ignited, the carbon residue is not less than 28.5%, the damage length after 15 times of water washing is not more than 14.3cm (the damage length of the polyester fabric before modification is 30cm, the dripping is 2-3 drops, the ignition absorbent cotton and the carbon residue are 13.2%), and the high-efficiency char-forming flame-retardant anti-dripping polyester fabric has excellent char forming performance and flame-retardant anti-dripping performance.
The principle of the invention is as follows:
in the prior art, chitosan and sodium alginate derived from bio-based polysaccharide are used as modifiers, and the polyester fabric is subjected to flame retardant modification by a layer-by-layer self-assembly technology driven by electrostatic acting force. However, sodium alginate has low thermal stability, metal oxide with high thermal stability cannot be formed, and meanwhile, the nitrogen content of chitosan is low, and the number of flammable polysaccharide groups is large, so that the flame retardant efficiency of a chitosan/sodium alginate system is poor, the flame retardant performance of a polyester fabric is not obviously improved, the modified polyester fabric is completely combusted in a vertical combustion test, and molten drops are generated.
The invention deposits cationic polyacrylamide, oxidized sodium alginate and parahydroxyben-zaldehyde on the surface of polyester fabric by a layer-by-layer self-assembly technology, and belongs to a halogen-free and phosphorus-free environment-friendly flame-retardant system. The cationic polyacrylamide molecular chain contains amino and amido, can be combined with aldehyde groups of oxidized sodium alginate and p-hydroxybenzaldehyde in a covalent bond manner, and can also be combined with the oxidized sodium alginate in an ionic bond manner to generate an insoluble coating which is deposited on the surface of the polyester fabric, so that a flame-retardant functional coating is formed on the surface of the polyester fabric;
the aromatic group of the parahydroxybenzaldehyde has higher thermal stability, the parahydroxybenzaldehyde is combined with the polysaccharide group of the oxidized sodium alginate in the thermal decomposition process to generate thermal stability carbon residue, and a compact carbon layer is formed on the surface of the polyester fabric, so that the effect of isolating heat and oxygen is achieved; in addition, the cationic polyacrylamide generates nonflammable nitrogen-containing gas in the heating process and plays a role in diluting the flammable gas. Therefore, the flame-retardant and anti-dripping performance of the coated polyester fabric can be improved through the synergistic effect formed among the aromatic group, the metal salt, the polysaccharide group and the nitrogen-containing group by the parahydroxybenzaldehyde, the oxidized sodium alginate and the cationic polyacrylamide, and the problem that the flame-retardant and anti-dripping performance of the halogen-free and phosphorus-free flame-retardant system in the prior art is poor for the polyester fabric is effectively solved.
Advantageous effects
The preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is simple and easy, improves the char formation performance and the flame-retardant anti-dripping performance of the polyester fabric, and solves the problem that the flame-retardant anti-dripping performance of the polyester fabric is poor by the existing halogen-free phosphorus-free flame-retardant system.
Drawings
FIG. 1 is a surface topography of a halogen-free, phosphorus-free flame retardant, anti-dripping polyester fabric (i.e., coated polyester fabric) and an uncoated polyester fabric of the present invention;
FIG. 2 is an infrared spectrum of a halogen-free, phosphorus-free flame retardant, anti-dripping polyester fabric (i.e., coated polyester fabric) and an uncoated polyester fabric of the present invention;
FIG. 3 is a vertical burn test chart of a halogen-free, phosphorus-free flame retardant, anti-dripping polyester fabric (i.e., coated polyester fabric) and an uncoated polyester fabric of the present invention.
Detailed Description
The invention is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The test methods involved in the following examples were:
weight gain rate: the weight gain rate of the coated fabric is the percentage of the mass difference between the coated fabric and the uncoated fabric to the mass of the uncoated fabric.
Damage length: the damage length of the fabric is measured according to GB/T5455-2014 standard of measurement of smoldering and continuous burning time of damage length of vertical direction of burning property of textile.
And (3) dripping: the molten drop of the fabric is measured according to GB/T5455-2014 standard of measurement of smoldering and continuous burning time of damage length of vertical direction of burning property of textile.
Carbon residue amount: the carbon residue of the fabric is the mass retention rate at 700 ℃ under the nitrogen condition in the thermal analysis test, and the heating rate is 10 ℃/min.
Damage length after 15 times of water washing: the washing method of the fabric is carried out by referring to AATCC 61-2006 accelerated test of washing fastness for household and commercial use, and the damage length is measured according to GB/T5455-2014 standard of measurement of smoldering and continuous burning time of damage length of textile in the vertical direction of burning performance.
In specific embodiments, the method for preparing oxidized sodium alginate is described in (He Shulan, zhang Min, geng Zhanjie, etc.. The method for preparing and performing partially oxidized sodium alginate [ J ]. Applied chemistry 2005, 22 (9): 1007-1011), specifically comprises the following steps:
(1) Dissolving sodium alginate in distilled water to prepare sodium alginate solution with the mass concentration of 2%;
(2) adding sodium periodate into the sodium alginate solution in the step (1) and oxidizing the sodium periodate at 30 ℃ in a dark place for 24 hours, wherein the molar ratio of the sodium periodate to the sodium alginate unit is 1:5,
(3) Adding glycol and sodium chloride into the oxidized solution in the step (2) to terminate the oxidation reaction, adding ethanol to precipitate, and performing suction filtration and ethanol washing to obtain oxidized sodium alginate; wherein the content of the ethylene glycol is 10wt% of the total solution after the ethylene glycol and the sodium chloride are added, and the content of the sodium chloride is 15wt% of the total solution after the ethylene glycol and the sodium chloride are added.
The oxidation degree of the prepared oxidized sodium alginate is 23%.
Example 1
The preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric comprises the following specific steps:
(1) Firstly, dissolving oxidized sodium alginate and parahydroxybenzaldehyde in a mixed solution of water and ethanol to obtain a mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, then soaking a polyester fabric in the mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment;
wherein the volume ratio of ethanol in the mixed solution of water and ethanol is 20%; in the mixed solution of oxidized sodium alginate and parahydroxyben-zaldehyde, the mass concentration of the oxidized sodium alginate is 1 percent, and the mass concentration of the parahydroxyben-zaldehyde is 2 percent; the rolling residual rate of the polyester fabric is 80%; the drying temperature is 70 ℃ and the drying time is 10min;
(2) Immersing the polyester fabric treated in the step (1) into a cationic polyacrylamide aqueous solution with the mass concentration of 1%, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment; wherein, the rolling surplus rate of the polyester fabric is 80%; the drying temperature is 70 ℃ and the drying time is 10min;
(3) And (3) alternately repeating the step (1) and the step (2) for 3 times to obtain the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric.
The prepared halogen-free and phosphorus-freeThe weight gain rate of the flame-retardant anti-dripping polyester fabric is 12.5 percent, and the carbon residue is 28.5 percent; as shown in fig. 1, the surface of the polyester fabric (i.e., the uncoated polyester fabric) was smooth, and the surface of the prepared halogen-free and phosphorus-free flame retardant anti-dripping polyester fabric (coated polyester fabric) was covered with a uniform flame retardant film, which indicates that oxidized sodium alginate, p-hydroxybenzaldehyde and cationic polyacrylamide were successfully deposited on the surface of the polyester fabric; as shown in fig. 2, the infrared spectrum of the coated polyester fabric shows many new absorption peaks compared to the uncoated polyester fabric; 3209cm -1 The broad absorption peak at the site is caused by the stretching vibration of the hydroxyl and amino groups; 2935cm -1 The absorption peak at the position is caused by the stretching vibration of the polysaccharide six-membered ring C-H; 1664 and 1406cm -1 The absorption peak at the position is caused by asymmetric and symmetric telescopic vibration of carboxyl; 1595cm -1 The absorption peak at the position is caused by the stretching vibration of the structure of Schiff base C=N; 1284cm -1 The absorption peak at the position is caused by the stretching vibration of C-C and C-O; 1216 and 1156cm -1 The absorption peak at the position is caused by the telescopic vibration of aldehyde group C-CHO; 1026cm -1 The absorption peak at the position is caused by the stretching vibration of C-O-C; the infrared spectrum result shows that oxidized sodium alginate, cationic polyacrylamide and p-hydroxy formaldehyde are successfully deposited on the surface of the polyester fabric, and the oxidized sodium alginate/p-hydroxy formaldehyde and the cationic polyacrylamide are crosslinked through Schiff base covalent bonds; as shown in fig. 3, the polyester fabric (i.e., uncoated polyester fabric) had poor flame retardant properties, and it completely burned in the vertical burning test, with a damage length of up to 30cm; the coated polyester fabric can self-extinguish in a vertical burning test, the damage length is 12.2cm, no molten drops are generated, and the coated polyester fabric has higher flame retardant property, and the damage length is 14.3cm after 15 times of water washing.
Example 2
The preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric comprises the following specific steps:
(1) Firstly, dissolving oxidized sodium alginate and parahydroxybenzaldehyde in a mixed solution of water and ethanol to obtain a mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, then soaking a polyester fabric in the mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment;
wherein the volume ratio of ethanol in the mixed solution of water and ethanol is 24%; in the mixed solution of oxidized sodium alginate and parahydroxyben-zaldehyde, the mass concentration of the oxidized sodium alginate is 1.4 percent, and the mass concentration of the parahydroxyben-zaldehyde is 2.4 percent; the rolling surplus rate of the polyester fabric is 84%; the drying temperature is 72 ℃ and the drying time is 9min;
(2) Immersing the polyester fabric treated in the step (1) into a cationic polyacrylamide aqueous solution with the mass concentration of 1.4%, taking out, removing excessive water on the fabric, and sequentially performing drying and water washing treatment; wherein, the rolling surplus rate of the polyester fabric is 84%; the drying temperature is 72 ℃ and the drying time is 9min;
(3) And (3) alternately repeating the step (1) and the step (2) for 4 times to obtain the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric.
The weight gain rate of the prepared halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 14.9%; the damage length of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 11.9cm, the dripping is 0 drop, the carbon residue amount is 29.1%, and the damage length after 15 times of water washing is 14cm.
Example 3
The preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric comprises the following specific steps:
(1) Firstly, dissolving oxidized sodium alginate and parahydroxybenzaldehyde in a mixed solution of water and ethanol to obtain a mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, then soaking a polyester fabric in the mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment;
wherein the volume ratio of ethanol in the mixed solution of water and ethanol is 28%; in the mixed solution of oxidized sodium alginate and parahydroxyben-zaldehyde, the mass concentration of the oxidized sodium alginate is 1.8 percent, and the mass concentration of the parahydroxyben-zaldehyde is 2.8 percent; the rolling surplus rate of the polyester fabric is 88%; the drying temperature is 74 ℃ and the drying time is 8min;
(2) Immersing the polyester fabric treated in the step (1) into a cationic polyacrylamide aqueous solution with the mass concentration of 1.8%, taking out, removing excessive water on the fabric, and sequentially performing drying and water washing treatment; wherein, the rolling surplus rate of the polyester fabric is 88%; the drying temperature is 74 ℃ and the drying time is 8min;
(3) And (3) alternately repeating the step (1) and the step (2) for 5 times to obtain the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric.
The weight gain rate of the prepared halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 16.1 percent; the damage length of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 11.2cm, the dripping is 0 drop, the carbon residue is 29.8%, and the damage length after 15 times of water washing is 13.5cm.
Example 4
The preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric comprises the following specific steps:
(1) Firstly, dissolving oxidized sodium alginate and parahydroxybenzaldehyde in a mixed solution of water and ethanol to obtain a mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, then soaking a polyester fabric in the mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment;
wherein the volume ratio of ethanol in the mixed solution of water and ethanol is 32%; in the mixed solution of oxidized sodium alginate and parahydroxyben-zaldehyde, the mass concentration of the oxidized sodium alginate is 2.2 percent, and the mass concentration of the parahydroxyben-zaldehyde is 3.2 percent; the rolling surplus rate of the polyester fabric is 92%; the drying temperature is 76 ℃ and the drying time is 7min;
(2) Immersing the polyester fabric treated in the step (1) into a cationic polyacrylamide aqueous solution with the mass concentration of 2.2%, taking out, removing excessive water on the fabric, and sequentially performing drying and water washing treatment; wherein, the rolling surplus rate of the polyester fabric is 92%; the drying temperature is 76 ℃ and the drying time is 7min;
(3) And (3) alternately repeating the step (1) and the step (2) for 6 times to obtain the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric.
The weight gain rate of the prepared halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 18.3 percent; the damage length of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 10.8cm, the dripping is 0 drop, the carbon residue is 30.3%, and the damage length after 15 times of water washing is 13.1cm.
Example 5
The preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric comprises the following specific steps:
(1) Firstly, dissolving oxidized sodium alginate and parahydroxybenzaldehyde in a mixed solution of water and ethanol to obtain a mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, then soaking a polyester fabric in the mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment;
wherein the volume ratio of ethanol in the mixed solution of water and ethanol is 36%; in the mixed solution of oxidized sodium alginate and parahydroxyben-zaldehyde, the mass concentration of the oxidized sodium alginate is 2.6 percent, and the mass concentration of the parahydroxyben-zaldehyde is 3.6 percent; the rolling surplus rate of the polyester fabric is 96%; the drying temperature is 78 ℃ and the drying time is 6min;
(2) Immersing the polyester fabric treated in the step (1) into a cationic polyacrylamide aqueous solution with the mass concentration of 2.6%, taking out, removing excessive water on the fabric, and sequentially performing drying and water washing treatment; wherein, the rolling surplus rate of the polyester fabric is 96%; the drying temperature is 78 ℃ and the drying time is 6min;
(3) And (3) alternately repeating the step (1) and the step (2) for 7 times to obtain the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric.
The weight gain rate of the prepared halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 20.4 percent; the damage length of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 10.2cm, the dripping is 0 drop, the carbon residue is 30.9%, and the damage length after 15 times of water washing is 12.7cm.
Example 6
The preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric comprises the following specific steps:
(1) Firstly, dissolving oxidized sodium alginate and parahydroxybenzaldehyde in a mixed solution of water and ethanol to obtain a mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, then soaking a polyester fabric in the mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment;
wherein the volume ratio of ethanol in the mixed solution of water and ethanol is 40%; in the mixed solution of oxidized sodium alginate and parahydroxyben-zaldehyde, the mass concentration of the oxidized sodium alginate is 3 percent, and the mass concentration of the parahydroxyben-zaldehyde is 4 percent; the rolling residual rate of the polyester fabric is 100%; the drying temperature is 80 ℃ and the drying time is 5min;
(2) Immersing the polyester fabric treated in the step (1) into a cationic polyacrylamide aqueous solution with the mass concentration of 3%, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment; wherein, the rolling surplus rate of the polyester fabric is 100%; the drying temperature is 80 ℃ and the drying time is 5min;
(3) And (3) alternately repeating the step (1) and the step (2) for 7 times to obtain the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric.
The weight gain rate of the prepared halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 21.2%; the damage length of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is 9.8cm, the dripping is 0 drop, the carbon residue amount is 31.4%, and the damage length after 15 times of water washing is 12.5cm.
Claims (9)
1. A preparation method of halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is characterized by comprising the following steps: and (3) depositing the cationic polyacrylamide, oxidized sodium alginate and parahydroxyben-zaldehyde on the surface of the polyester fabric by adopting a layer-by-layer self-assembly method to prepare the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric.
2. The method for preparing the halogen-free and phosphorus-free flame retardant anti-dripping polyester fabric according to claim 1, which is characterized by comprising the following specific steps:
(1) Firstly, dissolving oxidized sodium alginate and parahydroxybenzaldehyde in a mixed solution of water and ethanol to obtain a mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, then soaking a polyester fabric in the mixed solution of the oxidized sodium alginate and the parahydroxybenzaldehyde, taking out, removing excessive water on the fabric, and sequentially carrying out drying and washing treatment;
(2) Immersing the polyester fabric treated in the step (1) into cationic polyacrylamide aqueous solution, taking out, removing excessive water on the fabric, and sequentially performing drying and water washing treatment;
(3) And (3) alternately repeating the step (1) and the step (2) for a plurality of times to obtain the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric.
3. The preparation method of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is characterized in that in the mixed solution of oxidized sodium alginate and parahydroxyben-zaldehyde in the step (1), the mass concentration of the oxidized sodium alginate is 1-3%, and the mass concentration of the parahydroxyben-zaldehyde is 2-4%.
4. The preparation method of the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric is characterized in that the volume ratio of ethanol in the mixed liquid of water and ethanol in the step (1) is 20-40%.
5. The method for preparing the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric, according to claim 2, wherein the rolling allowance of the polyester fabric in the step (1) is 80-100%, the drying temperature is 70-80 ℃, and the drying time is 5-10 min.
6. The preparation method of the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric is characterized in that the mass concentration of the cationic polyacrylamide aqueous solution in the step (2) is 1-3%.
7. The method for preparing the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric, according to claim 2, wherein the rolling allowance of the polyester fabric in the step (2) is 80-100%, the drying temperature is 70-80 ℃, and the drying time is 5-10 min.
8. The method for preparing the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric, according to claim 2, is characterized in that the number of times of alternating repetition in the step (3) is 3-7, and the weight gain rate of the halogen-free and phosphorus-free flame-retardant anti-dripping polyester fabric is 12.5-21.2%.
9. The method for preparing the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric according to claim 2, wherein the damage length of the halogen-free phosphorus-free flame-retardant anti-dripping polyester fabric is not more than 12.2cm, the dripping is 0 drop, the carbon residue is not less than 28.5%, and the damage length after 15 times of water washing is not more than 14.3cm.
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