CN114737384B - Preparation method of polyester simulated silk fabric with lasting flame retardance - Google Patents
Preparation method of polyester simulated silk fabric with lasting flame retardance Download PDFInfo
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- 239000004744 fabric Substances 0.000 title claims abstract description 171
- 229920000728 polyester Polymers 0.000 title claims abstract description 153
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 230000002045 lasting effect Effects 0.000 title claims abstract description 35
- 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 claims abstract description 126
- 239000003063 flame retardant Substances 0.000 claims abstract description 118
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 42
- 239000011574 phosphorus Substances 0.000 claims abstract description 42
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000003513 alkali Substances 0.000 claims abstract description 25
- 208000016261 weight loss Diseases 0.000 claims abstract description 25
- 230000004048 modification Effects 0.000 claims abstract description 24
- 238000012986 modification Methods 0.000 claims abstract description 24
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000460 chlorine Substances 0.000 claims abstract description 21
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 21
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 14
- 230000004580 weight loss Effects 0.000 claims abstract description 13
- 239000013585 weight reducing agent Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 44
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 20
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 11
- BQTOJCOSKKLTAB-UHFFFAOYSA-L [Na+].O1P(OC1CO)(=O)OP(=O)([O-])[O-].[Na+] Chemical group [Na+].O1P(OC1CO)(=O)OP(=O)([O-])[O-].[Na+] BQTOJCOSKKLTAB-UHFFFAOYSA-L 0.000 claims description 6
- NABHFYBCCJNQKE-UHFFFAOYSA-M OOP(=O)(O)CC(=O)[O-].[Na+] Chemical compound OOP(=O)(O)CC(=O)[O-].[Na+] NABHFYBCCJNQKE-UHFFFAOYSA-M 0.000 claims 1
- 229920004933 Terylene® Polymers 0.000 abstract description 21
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 21
- 230000000052 comparative effect Effects 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
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- 238000010534 nucleophilic substitution reaction Methods 0.000 description 8
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- 238000012360 testing method Methods 0.000 description 6
- 238000000576 coating method Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
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- 230000001070 adhesive effect Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
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- 230000009471 action Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- IQEKRNXJPCBUAT-UHFFFAOYSA-N 2-[hydroperoxy(hydroxy)phosphoryl]acetic acid Chemical compound OOP(O)(=O)CC(O)=O IQEKRNXJPCBUAT-UHFFFAOYSA-N 0.000 description 1
- PVBVLSRHPABDLE-UHFFFAOYSA-N 2-phosphonoethaneperoxoic acid Chemical compound OOC(=O)CP(O)(O)=O PVBVLSRHPABDLE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 238000007730 finishing process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000037303 wrinkles Effects 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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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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
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/69—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with phosphorus; with halides or oxyhalides of phosphorus; with chlorophosphonic acid or its salts
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- 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
- D06M11/73—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 carbon or compounds thereof
- D06M11/76—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 carbon or compounds thereof with carbon oxides or carbonates
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- 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
- D06M13/288—Phosphonic or phosphonous acids or derivatives thereof
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- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/46—Compounds containing quaternary nitrogen atoms
- D06M13/463—Compounds containing quaternary nitrogen atoms derived from monoamines
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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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- 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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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a preparation method of a polyester simulated silk fabric with lasting flame retardance, which comprises the following steps of sequentially carrying out alkali decrement treatment, modification treatment and grafting treatment on the polyester fabric to prepare the polyester simulated silk fabric with lasting flame retardance; after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches more than 15wt%; the modification treatment process is a reaction process between hydroxyl on the surface of the polyester fabric and partial chlorine active groups of phosphorus oxychloride; the temperature of modification treatment is 30 to 40 ℃; the grafting treatment process is the reaction process between hydroxyl of the organic phosphorus-containing flame retardant and chlorine active groups on the surface of the polyester fabric. According to the method, a large number of flame-retardant groups are fixed on the terylene fabric through twice covalent grafting, so that the terylene imitated silk fabric has a high-efficiency durable flame-retardant function; the modified polyester simulated silk fabric has the advantages of high fire safety, good wearability, simple and convenient process flow, good application prospect of the product and high popularization value.
Description
Technical Field
The invention belongs to the technical field of textile functional finishing, and particularly relates to a preparation method of a durable flame-retardant polyester silk-like fabric.
Background
With the development of science and technology and the progress of textile industry, the development and application of textile products have a wider range. The terylene is the synthetic fiber with the fastest development speed, the highest yield and the widest application range in various synthetic fibers, and has the excellent characteristics of higher breaking strength and elastic modulus, moderate resilience, light resistance, heat resistance, corrosion resistance and the like. The polyester fabric has excellent wearability, stiffness and wrinkle resistance, and is widely used for clothes, curtains, bedding, interior decoration and various special materials. However, the terylene belongs to flammable fibers, the limit oxygen index of the terylene is only about 21 percent, the potential danger of fire is increasingly prominent along with the wide application of fiber fabrics, the terylene has very necessary flame retardant treatment, and has important practical significance and wide application prospect.
The terylene imitated silk fabric has soft hand feeling like silk, soft luster and comfortable wearing performance, and is widely applied. However, most of terylene silk-like fabrics are thin fabrics, and the burning is more violent, so that the terylene silk-like fabrics can meet the use requirements only by related flame-retardant finishing.
The phosphorus flame retardant has the characteristics of no halogen, environmental protection, high flame retardant efficiency and the like, and draws wide attention. The phosphorus flame retardant is heated and decomposed at high temperature to generate high-phosphoric acid substances with strong dehydration effect, so that the high polymer is carbonized to form a compact carbon layer to cover the surface and insulate oxygen and heat, and the dehydrated water absorbs heat to form steam, thereby reducing the temperature, diluting combustible gas and playing a role in flame retardance. At present, flame-retardant polyester fabrics are often developed through a textile after-finishing technology. Because the textile after-finishing technology has simple process and strong implementability, the influence of an addition method on the strong damage of the polyester fiber can be avoided. However, the polyester fiber does not have a reactive group that can react with the flame retardant, resulting in poor durability of the flame retardant finished polyester fabric.
In the document 1 (preparation and performance of flame-retardant coating adhesive for terylene [ J ] printing and dyeing, 2019, 45 (14): 1-6) and the document 2 (preparation and performance of flame-retardant coating process and flame-retardant performance [ J ] printing and dyeing, 2020, 46 (5): 1-7), an organic phosphorus flame retardant is mixed into aqueous polyacrylate and aqueous polyurethane coating adhesive to scrape and coat polyester fabrics, and the flame-retardant coating adhesive has better adhesion performance to the polyester fabrics and can improve the durability of the phosphorus flame retardant on the polyester fabrics, but the flame-retardant coating adhesive influences the air permeability and moisture permeability of the coating fabrics and cannot be applied to the terylene imitated silk fabrics.
Document 3 (flame retardant finishing process [ J ] of polyester flame retardant K-19. Printing and dyeing, 2010, 36 (21): 30-32) adopts a ring cage-shaped phosphonate flame retardant K-19 to improve the flame retardant property of polyester fabric through a rolling-drying-baking process, and the flame retardant polyester fabric has better water washing resistance, however, the method has higher baking temperature, influences the physical properties of the polyester simulated silk fabric, and has large energy consumption. The flame retardant can not be firmly combined with polyester fabric through covalent bonds.
Therefore, the research on the preparation method of the polyester simulated silk fabric with lasting flame retardance has very important significance for solving the problem of poor bonding property between the flame retardant and the fabric in the prior art.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a polyester silk-like fabric with lasting flame retardance.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a polyester silk-like fabric with lasting flame retardance comprises the following steps of sequentially carrying out alkali decrement treatment, modification treatment and grafting treatment on the polyester fabric to obtain the polyester silk-like fabric with lasting flame retardance;
after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches more than 15wt% (the weight loss is too little to achieve the silk-like effect), and meanwhile, hydroxyl is generated on the surface of the polyester fabric;
the modification treatment process is a reaction process between hydroxyl on the surface of the polyester fabric and partial chlorine active groups of phosphorus oxychloride; chlorine active groups can be introduced to the surface of the polyester fabric through modification treatment;
the temperature of the modification treatment is 30 to 40 ℃; the temperature of the invention is controlled within the range, so that the first chlorine active group and a small amount of the second chlorine active group of the phosphorus oxychloride react with the hydroxyl of the polyester fabric, the temperature rise is favorable for improving the nucleophilic substitution reaction efficiency, but the third chlorine active group is easy to react at an excessively high temperature, so that the phosphorus oxychloride loses activity and cannot react with the organic phosphorus-containing flame retardant subsequently;
the grafting treatment process is the reaction process between hydroxyl of the organic phosphorus-containing flame retardant and chlorine active groups on the surface of the polyester fabric; the grafting treatment can graft the organic phosphorus-containing flame retardant on the polyester fabric through covalent bonds.
As a preferred technical scheme:
according to the preparation method of the polyester simulated silk fabric with lasting flame retardance, alkali decrement treatment is carried out, namely the polyester fabric is immersed into a solution containing sodium hydroxide for treatment; wherein, sodium hydroxide is a terylene hydrolytic agent, and macromolecule chain segments on the surface of terylene are hydrolyzed under the action of sodium hydroxide.
The preparation method of the polyester simulated silk fabric with lasting flame retardance comprises the steps of enabling the concentration of sodium hydroxide in a solution containing the sodium hydroxide to be 5-10g/L; the concentration of sodium hydroxide is low, the efficiency of hydrolysis reaction of macromolecules on the surface of the terylene is low, the concentration is high, the hydrolysis efficiency is high, the waste is caused, the hydrolysis is serious, and the terylene fabric is damaged.
According to the preparation method of the durable flame-retardant polyester simulated silk fabric, the solution containing sodium hydroxide also contains hexadecyl trimethyl ammonium bromide; wherein, the hexadecyl trimethyl ammonium bromide is used as an accelerant to promote the hydrolysis reaction of the sodium hydroxide and the terylene.
According to the preparation method of the polyester simulated silk fabric with the lasting flame retardance, the concentration of the hexadecyl trimethyl ammonium bromide in the solution containing the sodium hydroxide is 0.5 to 1.5g/L; the concentration of the hexadecyl trimethyl ammonium bromide is low, the hydrolysis reaction efficiency of macromolecules on the surface of the terylene is low, the concentration is high, the hydrolysis efficiency is high, the waste is caused, the hydrolysis is serious, and the terylene fabric is damaged.
According to the preparation method of the durable flame-retardant polyester silk-like fabric, the temperature of alkali decrement treatment is 80-100 ℃, the time is 40-80min, and the bath ratio is 1; the higher the temperature is, the longer the time is, the more the polyester fabric hydrolysis is promoted, but the temperature is too high, the hydrolysis reaction is violent, and the polyester fabric is easily damaged; after the polyester fabric is treated at the temperature and for the time, the weight loss of the polyester fabric is 15 to 20wt%, so that the situation that the silk-like effect cannot be achieved due to too little weight loss is avoided, and the situation that the polyester fabric is seriously damaged due to too high weight loss is avoided.
According to the preparation method of the polyester simulated silk fabric with lasting flame retardance, modification treatment is carried out, namely the polyester fabric is immersed into an ethanol solution containing phosphorus oxychloride for treatment; phosphorus oxychloride can be hydrolyzed in water, so that ethanol is used as a solvent, and the ethanol is low in price and easy to obtain.
According to the preparation method of the lasting flame retardant polyester silk-like fabric, the concentration of phosphorus oxychloride in an ethanol solution containing the phosphorus oxychloride is 50 to 70g/L; the chlorine active group of the phosphorus oxychloride can perform nucleophilic substitution reaction with hydroxyl on the surface of the polyester fabric, a phosphorus-containing flame retardant group and a chlorine active group are introduced on the surface of the polyester fabric, the concentration of the phosphorus oxychloride is too low, sufficient chlorine active group and phosphorus-containing flame retardant group cannot be introduced, the concentration is too high, and the phosphorus oxychloride is saturated and is wasted.
According to the preparation method of the durable flame-retardant polyester silk-like fabric, the ethanol solution containing phosphorus oxychloride also contains sodium carbonate; the sodium carbonate plays a role in alkalescence, can neutralize acid generated by the nucleophilic substitution reaction, is beneficial to improving the reaction efficiency, and has small damage to the polyester fabric by adopting weak base.
According to the preparation method of the durable flame-retardant polyester silk-like fabric, the concentration of sodium carbonate in an ethanol solution containing phosphorus oxychloride is 15 to 25g/L; when the amount of sodium carbonate is too low, all the generated acid cannot be neutralized, and when the amount of sodium carbonate is too high, the waste is caused.
According to the preparation method of the durable flame-retardant polyester silk-like fabric, the time of modification treatment is 40-70min, and the bath ratio is 1.
According to the preparation method of the polyester simulated silk fabric with the lasting flame retardance, the polyester fabric is soaked in the ethanol solution containing the organic phosphorus-containing flame retardant for grafting treatment.
According to the preparation method of the durable flame-retardant polyester silk-like fabric, the molar ratio of the organic phosphorus-containing flame retardant used for grafting treatment to the phosphorus oxychloride used for modification treatment is 1 to 1.5; the residual active chlorine in the phosphorus oxychloride and the hydroxyl in the organic phosphorus-containing flame retardant are subjected to nucleophilic substitution reaction, the organic phosphorus-containing flame retardant is grafted on the surface of the polyester fabric, the concentration of the organic phosphorus-containing flame retardant is slightly excessive, so that the residual active chlorine in the phosphorus oxychloride completely participates in the reaction, and the residual active chlorine is saturated when the concentration is too high, thereby causing waste.
According to the preparation method of the durable flame-retardant polyester silk-like fabric, the organic phosphorus-containing flame retardant is sodium hydroxyethylidene diphosphate or 2-sodium hydroxyphosphonoacetate.
According to the preparation method of the polyester simulated silk fabric with lasting flame retardance, the ethanol solution containing the organic phosphorus-containing flame retardant also contains sodium carbonate; the sodium carbonate plays a role in alkalescence, neutralizes acid generated by the nucleophilic substitution reaction, contributes to improving the reaction efficiency, and causes less damage to the polyester fabric by adopting weak base.
According to the preparation method of the polyester silk-like fabric with the lasting flame retardance, the concentration of sodium carbonate in an ethanol solution containing the organic phosphorus-containing flame retardant is 15-25g/L, all generated acid cannot be neutralized if the using amount of the sodium carbonate is too low, and the waste is caused if the using amount of the sodium carbonate is too high.
According to the preparation method of the durable flame-retardant polyester silk-like fabric, the temperature of grafting treatment is 60-70 ℃, the time is 40-70min, and the bath ratio is 1; controlling the temperature within the range, so that residual chlorine active groups of phosphorus oxychloride react with hydroxyl groups of the organic phosphorus-containing flame retardant, and increasing the temperature is beneficial to improving the nucleophilic substitution reaction efficiency, but the boiling point of ethanol is considered, and the excessive high temperature causes waste; the high bath ratio is beneficial to the movement of the polyester fabrics in the finishing liquid, the finishing is more uniform, but the waste is caused when the bath ratio is too high.
According to the preparation method of the lasting flame-retardant polyester silk-like fabric, the damage length of the lasting flame-retardant polyester silk-like fabric is not more than 12.9cm, the damage length of the lasting flame-retardant polyester silk-like fabric is not more than 14.5cm after 20 times of washing, and the draping coefficient F of the lasting flame-retardant polyester silk-like fabric is not more than 38% (the draping coefficient of the untreated polyester fabric is 50%), which indicates that the lasting flame-retardant polyester silk-like fabric has lasting flame-retardant performance and better soft hand feeling.
The principle of the invention is as follows:
under the action of sodium hydroxide, hexadecyl trimethyl ammonium bromide and heat, polyethylene glycol terephthalate macromolecular chain segments on the surface of the polyester fabric are hydrolyzed, so that the surface of the polyester fabric is etched, the fabric is thinner and softer, has soft luster, and achieves the effect of silk-like; in addition, after hydrolysis etching, the surface of the polyester fabric contains a small amount of hydroxyl, so that a foundation is provided for durable flame-retardant finishing; under the condition of certain temperature, the first chlorine active group and part of the second chlorine active group and hydroxyl groups of the polyester fabric are subjected to nucleophilic substitution reaction, phosphorus-containing flame retardant groups are introduced to the surface of the polyester fabric through covalent bonds, and chlorine active groups with high reactivity are introduced to the surface of the polyester fabric, so that a foundation is provided for subsequently introducing more phosphorus-containing flame retardant groups; the residual chlorine active groups in the phosphorus oxychloride and hydroxyl groups in the organic phosphorus flame retardant, namely sodium hydroxyethylidene diphosphate or 2-hydroxyphosphonoacetate, have nucleophilic substitution reaction at a higher temperature, the organic phosphorus flame retardant is grafted on the polyester fabric through covalent bonds, and the phosphorus flame retardant groups are grafted on the polyester fabric through two reactions, so that the lasting flame retardant effect is achieved.
Advantageous effects
According to the method, the terylene fabric is endowed with a soft hand feeling and a certain active group through etching, and a large number of flame-retardant groups are fixed on the terylene fabric through twice covalent grafting, so that the terylene silk-like fabric is endowed with a high-efficiency and durable flame-retardant function. The modified polyester silk-like fabric has high fire safety and good wearability, the provided process flow is simple and convenient, the efficiency of functional modification is high, the application prospect of the product is good, and the product has high popularization value.
Drawings
Fig. 1 is a vertical burning test chart of a polyester simulated silk fabric with lasting flame retardance prepared in example 1.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The following examples and comparative examples relate to the following test methods:
the damage length of the fabric is measured according to the GB/T5455-2014 Standard of the determination of the smoldering and afterflame time of the damage length of the textile in the vertical direction of the combustion performance;
and (3) water washing resistance test: the washing method of the durable flame-retardant polyester silk-like fabric refers to AATCC 61-2006 accelerated test of washing fastness for household and commercial use.
Coefficient of drape F test: the drapability test of the durable flame-retardant polyester simulated silk fabric refers to the standard evaluation of GB/T23329-2009 'determination of the drapability of textile fabrics', and the drapability test has the advantages of small drapability coefficient, good drapability of the fabric and good hand feeling.
Example 1
A preparation method of a durable flame-retardant polyester simulated silk fabric comprises the following specific steps:
(1) Alkali decrement treatment;
immersing the polyester fabric into the solution a according to a bath ratio of 1; wherein the solution a consists of 5g/L of sodium hydroxide, 0.5g/L of hexadecyl trimethyl ammonium bromide and the balance of water;
after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches 15wt%;
(2) Modification treatment;
immersing the product obtained in the step (1) into the solution b according to a bath ratio of 1; wherein the solution b consists of 50g/L of phosphorus oxychloride, 15g/L of sodium carbonate and the balance of ethanol;
(3) Grafting treatment;
immersing the product obtained in the step (2) into the solution c according to a bath ratio of 1; wherein the solution c consists of an organic phosphorus-containing flame retardant (sodium hydroxyethylidene diphosphate), 15g/L of sodium carbonate and the balance of ethanol, and the molar ratio of the organic phosphorus-containing flame retardant to phosphorus oxychloride is 1:1.
The damage length of the finally prepared durable flame-retardant polyester silk-like fabric is 12.9cm (as shown in figure 1), the damage length is 14.5cm after 20 times of washing, and the drape coefficient F of the durable flame-retardant polyester silk-like fabric is 38%.
Comparative example 1
A method for preparing a flame-retardant polyester fabric, which is substantially the same as that of example 1, except that step (1) is omitted, and the untreated polyester fabric (the same as the raw material of example 1) is immersed in the solution b in step (2), i.e., the step of alkali weight reduction treatment is omitted in comparative example 1 with respect to example 1.
The damage length of the finally prepared flame-retardant polyester fabric is 13.1cm, the damage length is 30cm after 20 times of washing, and the draping coefficient F of the flame-retardant polyester fabric is 51%.
Comparing example 1 with comparative example 1, it can be seen that the flame-retardant polyester fabric of example 1 has better flame retardant performance and washing resistance and obtains soft hand feeling, but the flame-retardant polyester fabric of comparative example 1 has poorer washing resistance because the polyester fabric which is not subjected to alkali weight reduction treatment does not contain reactive groups and the flame retardant cannot be combined with the polyester fabric by covalent bonds.
Comparative example 2
A method for preparing a flame-retardant polyester silk-like fabric, which is substantially the same as example 1, except that step (2) is omitted, and the product of step (1) is immersed in the solution c in step (3) instead of the product of step (2), i.e., the step of modifying treatment is omitted in comparative example 2 with respect to example 1.
The damage length of the finally prepared flame-retardant polyester silk-like fabric is 13cm, the damage length is 30cm after 20 times of washing, and the suspension coefficient F of the flame-retardant polyester silk-like fabric is 37%.
Comparing example 1 with comparative example 2, it can be seen that the wash-resistant performance of the polyester fabric flame-retarded in comparative example 2 is poor, because the polyester fabric subjected to alkali weight reduction treatment only contains a small amount of active groups, and the flame retardant which generates covalent bonds with the polyester fabric is less, so that the flame-retardant effect is lost after washing.
Comparative example 3
A method for preparing a flame-retardant polyester silk-like fabric, which is substantially the same as example 1, except that step (3) is not included, i.e., step of grafting treatment is omitted in comparative example 3 with respect to example 1.
The damage length of the finally prepared flame-retardant polyester silk-like fabric is 18cm, the damage length is 30cm after 20 times of washing, and the draping coefficient F of the flame-retardant polyester silk-like fabric is 36%.
As can be seen by comparing the example 1 with the comparative example 3, the flame retardant performance and the water washing resistance of the polyester fabric which is flame retardant in the comparative example 3 are poor, because the content of the flame retardant on the polyester fabric which is not grafted by the phosphorus-containing flame retardant is low, and the flame retardant performance and the water washing resistance are poor.
Example 2
A preparation method of a polyester simulated silk fabric with lasting flame retardance comprises the following specific steps:
(1) Alkali decrement treatment;
immersing the polyester fabric into the solution a according to a bath ratio of 1; wherein the solution a consists of 6g/L of sodium hydroxide, 0.7g/L of hexadecyl trimethyl ammonium bromide and the balance of water;
after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches 16wt%;
(2) Modification treatment;
immersing the product obtained in the step (1) into the solution b according to the bath ratio of 1; wherein the solution b consists of 55g/L of phosphorus oxychloride, 17g/L of sodium carbonate and the balance of ethanol;
(3) Grafting treatment;
immersing the product obtained in the step (2) into the solution c according to the bath ratio of 1; wherein the solution c consists of an organic phosphorus-containing flame retardant (sodium hydroxyethylidene diphosphate), 17g/L of sodium carbonate and the balance of ethanol, and the molar ratio of the organic phosphorus-containing flame retardant to phosphorus oxychloride is 1.1.
The damage length of the finally prepared durable flame-retardant polyester silk-like fabric is 12.3cm, the damage length is 14cm after 20 times of washing, and the draping coefficient F of the durable flame-retardant polyester silk-like fabric is 35%.
Example 3
A preparation method of a polyester simulated silk fabric with lasting flame retardance comprises the following specific steps:
(1) Alkali decrement treatment;
immersing the polyester fabric into the solution a according to a bath ratio of 1; wherein the solution a consists of 7g/L of sodium hydroxide, 0.9g/L of hexadecyl trimethyl ammonium bromide and the balance of water;
after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches 17wt%;
(2) Modification treatment;
immersing the product obtained in the step (1) into the solution b according to the bath ratio of 1; wherein the solution b consists of 60g/L of phosphorus oxychloride, 19g/L of sodium carbonate and the balance of ethanol;
(3) Grafting treatment;
immersing the product obtained in the step (2) into the solution c according to the bath ratio of 1; wherein the solution c consists of an organic phosphorus-containing flame retardant (sodium hydroxyethylidene diphosphate), 19g/L of sodium carbonate and the balance of ethanol, and the molar ratio of the organic phosphorus-containing flame retardant to phosphorus oxychloride is 1.2.
The damage length of the finally prepared durable flame-retardant polyester silk-like fabric is 12cm, the damage length is 13.6cm after 20 times of washing, and the draping coefficient F of the durable flame-retardant polyester silk-like fabric is 33%.
Example 4
A preparation method of a durable flame-retardant polyester simulated silk fabric comprises the following specific steps:
(1) Alkali decrement treatment;
immersing the polyester fabric into the solution a according to a bath ratio of 1; wherein the solution a consists of 8g/L of sodium hydroxide, 1.1g/L of hexadecyl trimethyl ammonium bromide and the balance of water;
after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches 18wt%;
(2) Modification treatment;
immersing the product obtained in the step (1) into the solution b according to the bath ratio of 1; wherein the solution b consists of 65g/L of phosphorus oxychloride, 22g/L of sodium carbonate and the balance of ethanol;
(3) Grafting treatment;
immersing the product obtained in the step (2) into the solution c according to the bath ratio of 1; wherein the solution c consists of an organic phosphorus-containing flame retardant (2-sodium hydroxyphosphonoate) and the balance of ethanol, and the molar ratio of the organic phosphorus-containing flame retardant to phosphorus oxychloride is 1.3.
The damage length of the finally prepared durable flame-retardant polyester silk-like fabric is 11.4cm, the damage length of the fabric is 13cm after 20 times of washing, and the draping coefficient F of the durable flame-retardant polyester silk-like fabric is 30%.
Example 5
A preparation method of a durable flame-retardant polyester simulated silk fabric comprises the following specific steps:
(1) Alkali decrement treatment;
immersing the polyester fabric into the solution a according to a bath ratio of 1; wherein the solution a consists of 9g/L of sodium hydroxide, 1.5g/L of hexadecyl trimethyl ammonium bromide and the balance of water;
after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches 20wt%;
(2) Modification treatment;
immersing the product obtained in the step (1) into the solution b according to the bath ratio of 1; wherein the solution b consists of 70g/L of phosphorus oxychloride and the balance of ethanol;
(3) Grafting treatment;
immersing the product obtained in the step (2) into the solution c according to the bath ratio of 1; wherein the solution c consists of an organic phosphorus-containing flame retardant (2-sodium hydroxyphosphonoate), 22g/L of sodium carbonate and the balance of ethanol, and the molar ratio of the organic phosphorus-containing flame retardant to phosphorus oxychloride is 1.4.
The damage length of the finally prepared durable flame-retardant polyester silk-like fabric is 11.8cm, the damage length of the fabric is 13.3cm after 20 times of washing, and the draping coefficient F of the durable flame-retardant polyester silk-like fabric is 29%.
Example 6
A preparation method of a durable flame-retardant polyester simulated silk fabric comprises the following specific steps:
(1) Alkali decrement treatment;
immersing the polyester fabric into the solution a according to a bath ratio of 1; wherein the solution a consists of 10g/L of sodium hydroxide and the balance of water;
after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches 16wt%;
(2) Modification treatment;
immersing the product obtained in the step (1) into the solution b according to a bath ratio of 1; wherein the solution b consists of 70g/L of phosphorus oxychloride, 25g/L of sodium carbonate and the balance of ethanol;
(3) Grafting treatment;
immersing the product obtained in the step (2) into the solution c according to a bath ratio of 1; wherein the solution c consists of an organic phosphorus-containing flame retardant (2-sodium hydroxyphosphonoate), 25g/L of sodium carbonate and the balance of ethanol, and the molar ratio of the organic phosphorus-containing flame retardant to phosphorus oxychloride is 1.5.
The damage length of the finally prepared durable flame-retardant polyester silk-like fabric is 10.7cm, the damage length is 12.5cm after 20 times of washing, and the draping coefficient F of the durable flame-retardant polyester silk-like fabric is 35%.
Claims (10)
1. A preparation method of a polyester silk-like fabric with lasting flame retardance is characterized in that the polyester fabric is subjected to alkali decrement treatment, modification treatment and grafting treatment in sequence to prepare the polyester silk-like fabric with lasting flame retardance;
after the alkali weight reduction treatment, the weight loss of the polyester fabric reaches more than 15wt%;
the modification treatment process is a reaction process between hydroxyl on the surface of the polyester fabric and partial chlorine active groups of phosphorus oxychloride;
the temperature of modification treatment is 30 to 40 ℃;
the grafting treatment process is the reaction process between hydroxyl of the organic phosphorus-containing flame retardant and chlorine active groups on the surface of the polyester fabric.
2. The method for preparing the polyester silk-like fabric with lasting flame retardance according to claim 1, wherein the polyester fabric is immersed in a solution containing sodium hydroxide for alkali decrement treatment; the concentration of sodium hydroxide in the solution containing sodium hydroxide is 5-10g/L; the temperature of the alkali weight reduction treatment is 80-100 ℃, the time is 40-80min, and the bath ratio is 1.
3. The preparation method of the lasting flame-retardant polyester silk-like fabric according to claim 2, wherein the solution containing sodium hydroxide further contains 0.5 to 1.5g/L of cetyltrimethylammonium bromide.
4. The preparation method of the durable flame-retardant polyester silk-like fabric according to claim 1, wherein the modification treatment is carried out by immersing the polyester fabric into an ethanol solution containing phosphorus oxychloride; the concentration of phosphorus oxychloride in the ethanol solution containing the phosphorus oxychloride is 50 to 70g/L; the time of the modification treatment is 40 to 70min, and the bath ratio is 1.
5. The preparation method of the lasting flame retardant polyester silk-like fabric according to claim 4, wherein the ethanol solution containing phosphorus oxychloride further contains 15 to 25g/L of sodium carbonate.
6. The preparation method of the polyester silk-like fabric with lasting flame retardance according to claim 1, wherein the grafting treatment is carried out by immersing the polyester fabric into an ethanol solution containing an organic phosphorus-containing flame retardant; the temperature of the grafting treatment is 60 to 70 ℃, the time is 40 to 70min, and the bath ratio is 1.
7. The preparation method of the polyester silk-like fabric with lasting flame retardance as claimed in claim 6, wherein the molar ratio of the organic phosphorus-containing flame retardant used for grafting treatment to the phosphorus oxychloride used for modification treatment is 1 to 1.5.
8. The method for preparing the polyester silk-like fabric with lasting flame retardance according to claim 6, wherein the organic phosphorus-containing flame retardant is sodium hydroxyethylidene diphosphate or sodium 2-hydroxyphosphonoacetate.
9. The preparation method of the lasting flame retardant polyester silk-like fabric according to claim 6, wherein the ethanol solution containing the organic phosphorus-containing flame retardant further contains 15 to 25g/L of sodium carbonate.
10. The method for preparing the durable flame-retardant polyester silk-like fabric according to any one of claims 1~9, wherein the damaged length of the durable flame-retardant polyester silk-like fabric is not higher than 12.9cm, the damaged length of the durable flame-retardant polyester silk-like fabric is not higher than 14.5cm after 20 times of washing, and the drape coefficient F of the durable flame-retardant polyester silk-like fabric is not higher than 38%.
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| CH418294A (en) * | 1964-08-27 | 1967-02-15 | Geigy Ag J R | Process for dyeing and printing polyester fibers made from aromatic polycarboxylic acids and polyhydric alcohols |
| JP2001279576A (en) * | 2000-03-29 | 2001-10-10 | Nicca Chemical Co Ltd | Anti-yellowing finishing agent for textile material and finishing method |
| JP2003213144A (en) * | 2002-01-28 | 2003-07-30 | Teijin Chem Ltd | Flame-retardant thermoplastic resin composition |
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| CN108301100A (en) * | 2017-11-08 | 2018-07-20 | 江苏意瑞达纺织科技有限公司 | The manufacturing method of novel nano negative ion flame-retardant window shade cloth |
| CN107805936A (en) * | 2017-11-16 | 2018-03-16 | 江阴市博帆化纺有限公司 | A kind of method of modified polyester fibre |
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| CN113047031B (en) * | 2021-05-12 | 2022-03-11 | 苏州大学 | Durable flame-retardant low-smoke polyester fabric and preparation method thereof |
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