CN108978206A - A kind of preparation method of macromolecular graft modification inflaming retarding fabric - Google Patents

A kind of preparation method of macromolecular graft modification inflaming retarding fabric Download PDF

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Publication number
CN108978206A
CN108978206A CN201810721231.XA CN201810721231A CN108978206A CN 108978206 A CN108978206 A CN 108978206A CN 201810721231 A CN201810721231 A CN 201810721231A CN 108978206 A CN108978206 A CN 108978206A
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fabric
parts
solution
added
inflaming retarding
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李德喜
陈宗明
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Suzhou City Tianao Special Embroidery Co Ltd
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Suzhou City Tianao Special Embroidery Co Ltd
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Priority to CN201810721231.XA priority Critical patent/CN108978206A/en
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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
    • D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
    • 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
    • D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
    • D—TEXTILES; PAPER
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    • 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
    • D—TEXTILES; PAPER
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    • 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
    • D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
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    • 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
    • D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
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    • 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
    • D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/64—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 nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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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
    • D06M13/10—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
    • D06M13/144—Alcohols; Metal alcoholates
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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
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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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
    • D06M13/322—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
    • D06M13/325—Amines
    • D06M13/332—Di- or polyamines
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    • 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
    • D06M13/322—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
    • D06M13/372—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 containing etherified or esterified hydroxy groups ; Polyethers of low molecular weight
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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
    • 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
    • D06M13/322—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
    • D06M13/44—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 containing nitrogen and phosphorus
    • D06M13/453—Phosphates or phosphites containing nitrogen atoms
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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
    • D06M13/322—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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    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
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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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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Materials For Photolithography (AREA)

Abstract

The present invention provides a kind of preparation methods of macromolecular graft modification inflaming retarding fabric, fabric is respectively processed with alkaline solution and acid solution first, pentaerythritol triacrylate is aggregated in web surface again, obtain the fabric of surface grafting, it is handled again by ethylenediamine and is crosslinked Melamine Polyphosphate, then be immersed in finished product in the mixed solution being made of nano-aluminum hydroxide, dialkyl dimethyl quaternary ammonium salt, stearic acid diethanol amine, citric acid, chitosan, ethyl alcohol.Fabric limit oxygen index LOI produced by the present invention is greater than 40, has good flame retardant effect, while satisfactory mechanical property, and therefore, fabric produced by the present invention has important use value in inflaming retarding fabric field.

Description

A kind of preparation method of macromolecular graft modification inflaming retarding fabric
Technical field
The invention belongs to textile technology fields, and in particular to a kind of preparation method of macromolecular graft modification inflaming retarding fabric.
Background technique
The main reason for modern city skyscraper stands in great numbers, population high concentration, and inflammable textile becomes Urban Fires One of.According to the different purposes of textile, mechanical property and flame retardant property to fiber and its products propose tool for many countries The requirement of body defines the curtain of the public places such as old man, child, the clothes of disabled person and hospital, arenas, hotel, carpet is used Textile must all reach certain mechanical property and flame-retardant standard.Foreign countries are more early to the exploitation and research of flame-retardant textile, some Industrially developed country has just formulated the flame retardant regulation of textile early in mid-term the 1970s, and requires higher and higher, rule It is fixed increasingly thinner.China's also research and development in Efforts To Develop to flame retardant textiles in recent years, and achieved suitable progress.
However existing inflaming retarding fabric is arranged by finishing agent and has obtained flame retardant effect, however this processing mode Fastness to washing is poor, cannot obtain permanent flame retardant effect.
Summary of the invention
For the above problem of the existing technology, the purpose of the present invention is to provide a kind of macromolecular graft modification is fire-retardant The preparation method of fabric, to improve the flame retardant property of fabric.
To achieve the goals above, the present invention the following technical schemes are provided:
A kind of preparation method of macromolecular graft modification inflaming retarding fabric, comprising the following steps:
(1) fabric is immersed in the lye of 2-5%, in 25-35 DEG C of at a temperature of stir process under the revolving speed of 300-500r/min Fabric drying is washed 3-5 times with clear water, is then dipped in again in the acid solution of 3-5%, in 300-500r/min by 40-60min Revolving speed under at a temperature of 25-35 DEG C stir process 40-60min, fabric drying is washed with clear water to neutrality, drying drying It is spare afterwards；
(2) pentaerythritol triacrylate is added in DMF solvent and is configured to the solution that volume fraction is 10-30%, by step (1) fabric prepared immerses in the DMF solution of pentaerythritol triacrylate, and step (1) processing is added while stirring Fabric afterwards, is then added photoinitiator so that the volume fraction of photoinitiator be 5-10%, 30-50 DEG C at a temperature of continue It is stirred to react 12-24h, then takes out fabric, places it in and covers quartz plate on glass plate, is placed in ultraviolet light and carries out ultraviolet light Radiation grafting；After the completion of radiation, fabric taking-up is subjected to cleaning 2-3 times with DMF solution, then uses aqueous cleaning 2-3 times, obtains To the fabric of surface grafting；
(3) fabric for being grafted step (2) impregnation 4-8h in the ethylenediamine solution of 3-5%, then cleaned with deionized water, Then it is dipped in impregnation 5-10h in the Melamine Polyphosphate solution of 5-10% again, then is washed with deionized 3-5 times, fabric is dried after moisture is dried；
(4) PBS of the pH7.4 of the polyvinylpyrrolidone containing 5-10% of 5-10 times of parts by weight 100 parts of nano-aluminum hydroxide is added In buffer, 15-30 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicanes are added while stirring, in stirring Under the conditions of temperature risen to 50-70 DEG C, and this thermotonus 4-8h is kept, by the way that precipitating is collected by centrifugation, and clear with deionized water It washes 3-5 times, is finally dried for standby precipitating；
(5) by 12-20 parts of nano-aluminum hydroxide made from step (4), 8-15 parts of dialkyl dimethyl quaternary ammonium salt, stearic acid diethyl 5-10 parts of hydramine, 6-13 parts of citric acid, 7-14 parts of chitosan, 20-40 parts of ethyl alcohol be mixed, after mixing evenly by step (3) impregnation 3-5h in mixed solution is added in the fabric handled, then takes out fabric and dries, and is placed in drying in baking oven and is made Finished product.
Preferably, the lye in the step (1) is NaOH, KOH, NaHCO3The lye of configuration, in the step (1) Acid solution is HCl, HNO3、H2SO4The acid solution of configuration.
Preferably, the photoinitiator in the step (2) is benzophenone.
Preferably, in the radiation operations in the step (2) web surface away from light source 53mm, radiated time 15-30min.
Preferably, the parts by weight of each raw material in the step (5) are 16 parts of nano-aluminum hydroxide, dialkyl dimethyl season 12 parts of ammonium salt, 7 parts of stearic acid diethanol amine, 10 parts of citric acid, 10 parts of chitosan, 30 parts of ethyl alcohol.
The utility model has the advantages that the present invention provides a kind of preparation methods of macromolecular graft modification inflaming retarding fabric, by fabric Surface grafting large biological molecule, web surface formed cross-linked network structure, then with have flame retardant property melamine poly Phosphate and nano-aluminum hydroxide crosslinking are handled fabric in web surface, then with other function raw material, are had The fabric of good flame-retardance energy.Fabric limit oxygen index LOI produced by the present invention is greater than 40, has good flame retardant effect, together When satisfactory mechanical property, therefore, fabric produced by the present invention inflaming retarding fabric field have important use value.
Specific embodiment
The invention will now be further described with reference to specific embodiments, but examples are merely exemplary, not to this hair Bright range constitutes any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention Can with the details and forms of the technical scheme of the invention are modified or replaced, but these modification and replacement each fall within it is of the invention In protection scope.
Embodiment 1
A kind of preparation method of macromolecular graft modification inflaming retarding fabric, comprising the following steps:
(1) fabric is immersed in 3.5% lye, in 30 DEG C of at a temperature of stir process 50min under the revolving speed of 400r/min, Fabric drying is washed 3-5 times with clear water, is then dipped in again in 4% acid solution, in 30 DEG C under the revolving speed of 400r/min At a temperature of stir process 50min, fabric drying is washed with clear water to neutrality, it is spare after drying drying；
(2) pentaerythritol triacrylate is added in DMF solvent and is configured to the solution that volume fraction is 20%, step (1) is made Standby fabric immerses in the DMF solution of pentaerythritol triacrylate, is added step (1) while stirring treated face Material, then be added photoinitiator benzophenone so that the volume fraction of photoinitiator be 7%, 40 DEG C at a temperature of continue to stir 18h is reacted, fabric is then taken out, places it in and cover quartz plate on glass plate, progress ultraviolet radiation in ultraviolet light is placed in and connects Branch；After the completion of radiation, fabric taking-up is subjected to cleaning 2-3 times with DMF solution, then uses aqueous cleaning 2-3 times, obtains surface The fabric of grafting；
(3) fabric for being grafted step (2) impregnation 6h in 4% ethylenediamine solution, then cleaned with deionized water, then It is dipped in impregnation 7.5h in 7% Melamine Polyphosphate solution again, then is washed with deionized 3-5 times, it will Fabric is dried after moisture drying；
(4) PBS buffer solution of the pH7.4 containing 8% polyvinylpyrrolidone of 8 times of parts by weight 100 parts of nano-aluminum hydroxide is added In, 23 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicanes are added while stirring, it under stirring conditions will be warm Degree rises to 60 DEG C, and keeps this thermotonus 6h, by the way that precipitating is collected by centrifugation, and is cleaned 3-5 times with deionized water, will finally be sunk Shallow lake is dried for standby；
(5) by 16 parts of nano-aluminum hydroxide made from step (4), 12 parts of dialkyl dimethyl quaternary ammonium salt, stearic acid diethanol amine 7 Part, 10 parts of citric acid, 10 parts of chitosan, 30 parts of ethyl alcohol be mixed, after mixing evenly by step (3) handle fabric add Enter impregnation 3-5h in mixed solution, then fabric is taken out and is dried, is placed in baking oven and dries finished product.
Lye in the step (1) is the lye of NaOH configuration, and the acid solution in the step (1) is the acid of HCl configuration Liquid.
Web surface is away from light source 53mm, radiated time 23min in radiation operations in the step (2).
Embodiment 2
A kind of preparation method of macromolecular graft modification inflaming retarding fabric, comprising the following steps:
(1) fabric is immersed in 2% lye, it, will in 25 DEG C of at a temperature of stir process 40min under the revolving speed of 300r/min Fabric drying is washed 3-5 times with clear water, is then dipped in again in 3% acid solution, in 25 DEG C of temperature under the revolving speed of 300r/min Lower stir process 40min is spent, fabric drying is washed with clear water to neutrality, it is spare after drying drying；
(2) pentaerythritol triacrylate is added in DMF solvent and is configured to the solution that volume fraction is 10%, step (1) is made Standby fabric immerses in the DMF solution of pentaerythritol triacrylate, is added step (1) while stirring treated face Material, then be added photoinitiator benzophenone so that the volume fraction of photoinitiator be 5%, 30 DEG C at a temperature of continue to stir 12h is reacted, fabric is then taken out, places it in and cover quartz plate on glass plate, progress ultraviolet radiation in ultraviolet light is placed in and connects Branch；After the completion of radiation, fabric taking-up is subjected to cleaning 2-3 times with DMF solution, then uses aqueous cleaning 2-3 times, obtains surface The fabric of grafting；
(3) fabric for being grafted step (2) impregnation 4h in 3% ethylenediamine solution, then cleaned with deionized water, then It is dipped in impregnation 5h in 5% Melamine Polyphosphate solution again, then is washed with deionized 3-5 times, by water Fabric is dried after dividing drying；
(4) PBS buffer solution of the pH7.4 containing 5% polyvinylpyrrolidone of 5 times of parts by weight 100 parts of nano-aluminum hydroxide is added In, 15 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicanes are added while stirring, it under stirring conditions will be warm Degree rises to 50 DEG C, and keeps this thermotonus 4h, by the way that precipitating is collected by centrifugation, and is cleaned 3-5 times with deionized water, will finally be sunk Shallow lake is dried for standby；
(5) by 12 parts of nano-aluminum hydroxide made from step (4), 8 parts of dialkyl dimethyl quaternary ammonium salt, stearic acid diethanol amine 5 Part, 6 parts of citric acid, 7 parts of chitosan, 20 parts of ethyl alcohol be mixed, after mixing evenly by step (3) processing fabric be added Then fabric is taken out and is dried, is placed in baking oven and dry finished product by impregnation 3h in mixed solution.
Lye in the step (1) is NaHCO3The lye of configuration, the acid solution in the step (1) are H2SO4Configuration Acid solution.
Web surface is away from light source 53mm, radiated time 15min in radiation operations in the step (2).
Embodiment 3
A kind of preparation method of macromolecular graft modification inflaming retarding fabric, comprising the following steps:
(1) fabric is immersed in 3% lye, it, will in 28 DEG C of at a temperature of stir process 45min under the revolving speed of 350r/min Fabric drying is washed 3-5 times with clear water, is then dipped in again in 3.5% acid solution, in 26 DEG C under the revolving speed of 350r/min At a temperature of stir process 45min, fabric drying is washed with clear water to neutrality, it is spare after drying drying；
(2) pentaerythritol triacrylate is added in DMF solvent and is configured to the solution that volume fraction is 15%, step (1) is made Standby fabric immerses in the DMF solution of pentaerythritol triacrylate, is added step (1) while stirring treated face Material, then be added photoinitiator benzophenone so that the volume fraction of photoinitiator be 6%, 35 DEG C at a temperature of continue to stir 15h is reacted, fabric is then taken out, places it in and cover quartz plate on glass plate, progress ultraviolet radiation in ultraviolet light is placed in and connects Branch；After the completion of radiation, fabric taking-up is subjected to cleaning 2-3 times with DMF solution, then uses aqueous cleaning 2-3 times, obtains surface The fabric of grafting；
(3) fabric for being grafted step (2) impregnation 5h in 3.5% ethylenediamine solution, then cleaned with deionized water, so It is dipped in impregnation 6h in 7% Melamine Polyphosphate solution again afterwards, then is washed with deionized 3-5 times, it will Fabric is dried after moisture drying；
(4) PBS buffer solution of the pH7.4 containing 6% polyvinylpyrrolidone of 7 times of parts by weight 100 parts of nano-aluminum hydroxide is added In, 20 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicanes are added while stirring, it under stirring conditions will be warm Degree rises to 55 DEG C, and keeps this thermotonus 5h, by the way that precipitating is collected by centrifugation, and is cleaned 3-5 times with deionized water, will finally be sunk Shallow lake is dried for standby；
(5) by 14 parts of nano-aluminum hydroxide made from step (4), 10 parts of dialkyl dimethyl quaternary ammonium salt, stearic acid diethanol amine 6 Part, 8 parts of citric acid, 9 parts of chitosan, 25 parts of ethyl alcohol be mixed, after mixing evenly by step (3) processing fabric be added Then fabric is taken out and is dried, is placed in baking oven and dry finished product by impregnation 3.5h in mixed solution.
Preferably, the lye in the step (1) is the lye of KOH configuration, and the acid solution in the step (1) is HNO3Match The acid solution set.
Web surface is away from light source 53mm, radiated time 18min in radiation operations in the step (2).
Embodiment 4
A kind of preparation method of macromolecular graft modification inflaming retarding fabric, comprising the following steps:
(1) fabric is immersed in 5% lye, it, will in 35 DEG C of at a temperature of stir process 60min under the revolving speed of 500r/min Fabric drying is washed 5 times with clear water, is then dipped in again in 5% acid solution, in 35 DEG C of temperature under the revolving speed of 500r/min Lower stir process 60min washs fabric drying to neutrality with clear water, spare after drying drying；
(2) pentaerythritol triacrylate is added in DMF solvent and is configured to the solution that volume fraction is 30%, step (1) is made Standby fabric immerses in the DMF solution of pentaerythritol triacrylate, is added step (1) while stirring treated face Material, then be added photoinitiator benzophenone so that the volume fraction of photoinitiator be 10%, 50 DEG C at a temperature of continue to stir It mixes reaction for 24 hours, then takes out fabric, place it in and cover quartz plate on glass plate, be placed in ultraviolet light and carry out ultraviolet radiation Grafting；After the completion of radiation, fabric taking-up is subjected to cleaning 2-3 times with DMF solution, then uses aqueous cleaning 2-3 times, obtains table The fabric of face grafting；
(3) fabric for being grafted step (2) impregnation 8h in 5% ethylenediamine solution, then cleaned with deionized water, then It is dipped in impregnation 10h in 10% Melamine Polyphosphate solution again, then is washed with deionized 3-5 times, it will Fabric is dried after moisture drying；
(4) PBS for the pH7.4 containing 10% polyvinylpyrrolidone that 100 parts of nano-aluminum hydroxide are added 10 times of parts by weight is buffered In liquid, 30 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicanes are added while stirring, under stirring conditions will Temperature rises to 70 DEG C, and keeps this thermotonus 8h, by the way that precipitating is collected by centrifugation, and is cleaned 5 times with deionized water, will finally be sunk Shallow lake is dried for standby；
(5) by 20 parts of nano-aluminum hydroxide made from step (4), 15 parts of dialkyl dimethyl quaternary ammonium salt, stearic acid diethanol amine 10 parts, 13 parts of citric acid, 14 parts of chitosan, 40 parts of ethyl alcohol be mixed, after mixing evenly by step (3) handle fabric Impregnation 5h in mixed solution is added, then fabric is taken out and is dried, is placed in baking oven and dries finished product.
Preferably, the lye in the step (1) is NaHCO3The lye of configuration, the acid solution in the step (1) are H2SO4The acid solution of configuration.
Web surface is away from light source 53mm, radiated time 30min in radiation operations in the step (2).
Fabric made from embodiment 1-4 is measured referring to GB/T5454-1997 textile combustion performance test oxygen index method The limit oxygen index of fabric evaluates the anti-flammability of fabric；It " textile fabric ultimate strength and is stretched referring to ASTM D 5035- 2003 Long standard test method (galley proof method) " measurement fabric breaking strength, test result is as shown in table 1, obtained from table 1, this It invents fabric limit oxygen index LOI obtained and is greater than 40, there is good flame retardant effect, while satisfactory mechanical property, therefore, this Inventing fabric obtained has important use value table 1 in inflaming retarding fabric field

Claims (5)

1. a kind of preparation method of macromolecular graft modification inflaming retarding fabric, which comprises the following steps:
(1) fabric is immersed in the lye of 2-5%, in 25-35 DEG C of at a temperature of stir process under the revolving speed of 300-500r/min Fabric drying is washed 3-5 times with clear water, is then dipped in again in the acid solution of 3-5%, in 300-500r/min by 40-60min Revolving speed under at a temperature of 25-35 DEG C stir process 40-60min, fabric drying is washed with clear water to neutrality, drying drying It is spare afterwards；
(2) pentaerythritol triacrylate is added in DMF solvent and is configured to the solution that volume fraction is 10-30%, by step (1) fabric prepared immerses in the DMF solution of pentaerythritol triacrylate, and step (1) processing is added while stirring Fabric afterwards, is then added photoinitiator so that the volume fraction of photoinitiator be 5-10%, 30-50 DEG C at a temperature of continue It is stirred to react 12-24h, then takes out fabric, places it in and covers quartz plate on glass plate, is placed in ultraviolet light and carries out ultraviolet light Radiation grafting；After the completion of radiation, fabric taking-up is subjected to cleaning 2-3 times with DMF solution, then uses aqueous cleaning 2-3 times, obtains To the fabric of surface grafting；
(3) fabric for being grafted step (2) impregnation 4-8h in the ethylenediamine solution of 3-5%, then cleaned with deionized water, Then it is dipped in impregnation 5-10h in the Melamine Polyphosphate solution of 5-10% again, then is washed with deionized 3-5 times, fabric is dried after moisture is dried；
(4) PBS of the pH7.4 of the polyvinylpyrrolidone containing 5-10% of 5-10 times of parts by weight 100 parts of nano-aluminum hydroxide is added In buffer, 15-30 parts of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicanes are added while stirring, in stirring Under the conditions of temperature risen to 50-70 DEG C, and this thermotonus 4-8h is kept, by the way that precipitating is collected by centrifugation, and clear with deionized water It washes 3-5 times, is finally dried for standby precipitating；
(5) by 12-20 parts of nano-aluminum hydroxide made from step (4), 8-15 parts of dialkyl dimethyl quaternary ammonium salt, stearic acid diethyl 5-10 parts of hydramine, 6-13 parts of citric acid, 7-14 parts of chitosan, 20-40 parts of ethyl alcohol be mixed, after mixing evenly by step (3) impregnation 3-5h in mixed solution is added in the fabric handled, then takes out fabric and dries, and is placed in drying in baking oven and is made Finished product.
2. a kind of preparation method of macromolecular graft modification inflaming retarding fabric according to claim 1, which is characterized in that described Lye in step (1) is NaOH, KOH, NaHCO3The lye of configuration, the acid solution in the step (1) are HCl, HNO3、H2SO4 The acid solution of configuration.
3. a kind of preparation method of macromolecular graft modification inflaming retarding fabric according to claim 1, which is characterized in that described Photoinitiator in step (2) is benzophenone.
4. a kind of preparation method of macromolecular graft modification inflaming retarding fabric according to claim 1, which is characterized in that described Web surface is away from light source 53mm, radiated time 15-30min in radiation operations in step (2).
5. a kind of preparation method of macromolecular graft modification inflaming retarding fabric according to claim 1, which is characterized in that described The parts by weight of each raw material in step (5) are 16 parts of nano-aluminum hydroxide, 12 parts of dialkyl dimethyl quaternary ammonium salt, stearic acid diethyl 7 parts of hydramine, 10 parts of citric acid, 10 parts of chitosan, 30 parts of ethyl alcohol.
CN201810721231.XA 2018-07-04 2018-07-04 A kind of preparation method of macromolecular graft modification inflaming retarding fabric Pending CN108978206A (en)

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