CN112813685A - Durable flame-retardant after-finishing fabric and preparation method thereof - Google Patents
Durable flame-retardant after-finishing fabric and preparation method thereof Download PDFInfo
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- CN112813685A CN112813685A CN202010620333.XA CN202010620333A CN112813685A CN 112813685 A CN112813685 A CN 112813685A CN 202010620333 A CN202010620333 A CN 202010620333A CN 112813685 A CN112813685 A CN 112813685A
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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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- 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
- D06M14/26—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 on to materials of synthetic origin
- D06M14/30—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 on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/34—Polyamides
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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
- D06M11/07—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 System
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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
- D06M11/07—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
- D06M11/28—Halides of elements of Groups 8, 9, 10 or 18 of the Periodic System
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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
- D06M11/51—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
- D06M11/57—Sulfates or thiosulfates of elements of Groups 3 or 13 of the Periodic System, e.g. alums
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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
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- 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
- D06M14/26—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 on to materials of synthetic origin
- D06M14/30—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 on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/32—Polyesters
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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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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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
Abstract
The invention provides a durable flame-retardant after-finishing fabric and a preparation method thereof, belonging to the technical field of flame-retardant after-finishing of fabrics. The durable flame-retardant after-finishing fabric is prepared by combining the light grafting modification technology with the coordination anchoring effect of metal ions and grafting ligands, namely, the flame-retardant efficiency and the melt-drip resistance of the fabric are improved by adopting a method of carrying out a coordination reaction on the surface of the fabric on grafting ligand groups and introducing metal ions through the flame-retardant effect of the metal ions or the synergistic effect of the metal ions and flame-retardant elements (such as N elements) on a light grafting chain; meanwhile, the coordination crosslinking function between metal ions and ligand groups on the photo-grafting chain segment is utilized to improve the flame retardant durability of the photo-grafting chain segment. The data of the embodiment shows that the durable flame-retardant fabric prepared by the invention has better flame-retardant property and excellent durable property.
Description
Technical Field
The invention relates to the technical field of fabric flame-retardant after-finishing, in particular to durable flame-retardant after-finishing fabric and a preparation method thereof.
Background
The ultraviolet surface grafting modification adopts low-energy long-wave ultraviolet light as an irradiation source, grafting occurs at the depth of 50-100 nm on the surface or subsurface, the performance of a base material is not influenced in the modification process, and the ultraviolet surface grafting modification is applied to the flame-retardant after-finishing of fabrics at present. Chinese patents 'a durable flame-retardant after-finishing method for fabric (CN 101831804A)' and 'a post-finishing flame-retardant method for nylon fabric (CN 101831803A)' respectively take Acrylamide (AM) and 2-hydroxyethyl methacrylate phosphate as photosensitive monomers to carry out photo-grafting flame-retardant modification on PA fabric. However, researches show that although the flame-retardant photosensitive monomer can be covalently anchored on the surface of the fabric by the photo-grafting surface modification technology, most of the photosensitive monomers have limited flame-retardant effect, and the flame-retardant efficiency needs to be improved by increasing the grafting degree and increasing the content of flame-retardant groups on the modified fabric or carrying out secondary reaction with phosphorus and nitrogen compounds. Ren (Renyl, GuYT, ethyl, UV-induced surface grafting polymerization, phosphorus-crosslinking, polyester, polyamide, J.,2017,94:1-10.) and the like are photo-grafted on the PAn by hydroxyethyl acrylate (HEMA) and then react with phosphoric acid and urea to prepare the flame-retardant PAn fabric; yu (Yu LH, Zhang S, et al, ethylene, Impr ovingthe flame retardant polyester fabric, PETFA textile, Degrad, Stabil, 2010,95, 1934-sodium diphosphonic acid) and the like react Glycidyl Methacrylate (GMA) photograft modified PET fabric with hydroxyethylidene diphosphonic acid at high temperature to improve the flame retardant property of the fabric. But the hand feeling, appearance and body performance of the fabric are easily reduced, so that the characteristics of mild surface photo-grafting reaction condition and small damage to a base material lose significance; in a washing resistance test, the solvent, the alkaline environment and repeated mechanical force action also easily cause the breakage of the photograft chain, so that the durability efficiency of the modified flame-retardant fabric is low. Specifically, in the above patent, the fabric of acrylamide grafted photosensitive monomer has lower flame retardant effect oxygen index and poorer flame retardant and washing resistance; the 2-hydroxyethyl methacrylate phosphate grafted photosensitive monomer has poor hand feeling after finishing the fabric, and the practicability is limited, and the method for improving the flame retardant efficiency of the fabric through the secondary reaction of the photografting modified fabric and the high-efficiency flame retardant monomer containing elements such as phosphorus, nitrogen and the like is mostly carried out under the high-temperature condition, so that the performance of the fabric body is obviously reduced, and the advantages of the photografting surface modified fabric are greatly weakened.
Therefore, if the technical advantage that the performance of the fabric body is slightly damaged by photo-grafting flame-retardant modification can be utilized, the flame-retardant efficiency and durability of the modified fabric are further improved, and the preparation of the durable flame-retardant modified PA fabric is of great significance.
Disclosure of Invention
The invention aims to provide a durable flame-retardant after-finishing fabric and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of durable flame-retardant after-finishing fabric, which comprises the following steps:
soaking the fabric in a photosensitive monomer finishing liquid, and performing first padding finishing to obtain a padded fabric;
carrying out a photo-grafting reaction on the padded fabric to obtain a photo-grafted modified fabric;
and soaking the photo-grafting modified fabric in a metal salt finishing solution, and performing second padding finishing to obtain the durable flame-retardant after-finishing fabric.
Preferably, the fabric comprises cotton fabric, polyester fabric, nylon fabric, acrylic fabric or polyacrylonitrile fabric.
Preferably, the photosensitive monomer finishing liquid comprises a photosensitive monomer, a photocrosslinking agent, a photoinitiator and a solvent, wherein the photosensitive monomer comprises acrylamide, methacrylamide or acrylic acid; the photocrosslinking agent is N, N' -methylene bisacrylamide; the photoinitiator comprises benzophenone, 1- [4- (2-hydroxyethoxy) -phenylene ] -2-hydroxy-2 ', 2' -dimethyl ethyl ketone or 2-hydroxy-2-toluene-1-phenyl-1-acetone; the solvent is deionized water or acetone.
Preferably, in the photosensitive monomer finishing liquid, the mass fraction of the photosensitive monomer is 10-30%, and the mass fraction of the photocrosslinking agent is 0.5-5.0%; the mass fraction of the photoinitiator is 0.5-3.0%.
Preferably, the soaking time of the first padding finishing is 20 min-1 h, the rotating speed of a rolling mill is 0.2m/s, and the pressure is 0.5-1.0 MPa.
Preferably, the ultraviolet lamp intensity of the photografting reaction is 100W/cm2The irradiation time is 15-40 min, and the irradiation height is 5-30 cm.
Preferably, the metal salt finishing liquid comprises metal salt, a pH regulator and water; the metal salt comprises water-soluble calcium salt, zinc salt, aluminum salt, ferrous salt, ferric salt or copper salt; the pH regulator comprises sodium carbonate, hydrochloric acid or ammonium chloride.
Preferably, in the metal salt finishing liquid, the concentration of the metal salt is 0.5-3.0 mol/L, and the concentration of the pH regulator is 0.5-5 g/L.
Preferably, the soaking time of the second padding finishing is 20 min-1 h, the rotating speed of a rolling mill is 0.2m/s, and the pressure is 0.5-1.0 MPa.
The invention provides durable flame-retardant after-finishing fabric prepared by the preparation method in the technical scheme.
The invention provides a preparation method of durable flame-retardant after-finishing fabric, which comprises the following steps: soaking the fabric in a photosensitive monomer finishing liquid, and performing first padding finishing to obtain a padded fabric; carrying out a photo-grafting reaction on the padded fabric to obtain a photo-grafted modified fabric; and soaking the photo-grafting modified fabric in a metal salt finishing solution, and performing second padding finishing to obtain the durable flame-retardant after-finishing fabric.
The durable flame-retardant after-finishing fabric is prepared by combining the light grafting modification technology with the coordination anchoring effect of metal ions and grafting ligands for the first time, namely, the flame-retardant efficiency and the melt-drip resistance of the fabric are improved by adopting a method of carrying out a coordination reaction on the surface of the fabric on grafting ligand groups and introducing metal ions through the flame-retardant effect of the metal ions or the synergistic interaction of the metal ions and flame-retardant elements (such as N elements) on a light grafting chain; meanwhile, coordination crosslinking action is generated between the metal ions and the ligand groups on the photo-grafting chain segment, so that a coordination crosslinking structure with excellent structural stability is formed between the metal ions and the ligand groups on the photo-grafting chain segment, and the flame retardance and durability of the fabric are improved. The data of the embodiment shows that the durable flame-retardant fabric prepared by the invention has good flame retardant property and excellent durability, the oxygen index of the finished fabric can reach 36.8, the fabric does not have a molten drop phenomenon during combustion, and the oxygen index can be kept at about 29.0 after washing.
The method disclosed by the invention relates to two steps of an ultraviolet light surface grafting modification reaction and a metal ion coordination reaction, the conditions of the two reactions are mild, and a high-temperature baking process (the baking temperature of the traditional padding-baking flame-retardant post-finishing process is 160-200 ℃) which is easy to influence a material body in the traditional fabric durable flame-retardant finishing process is avoided, so that the influence on various properties of a base material body is small; meanwhile, the method has the characteristics of simple process, environmental protection, no toxicity, no pollution, economic price, easy industrial popularization and the like in the normal-temperature operation, finishing and using processes, can further expand the application of the optical grafting modification technology in the flame-retardant after-finishing field, promotes the development of the flame-retardant textile industry, and has important theoretical significance and practical value for realizing the green and environment-friendly development trend of the flame-retardant after-finishing process.
Compared with other durable flame-retardant after-finishing methods for fabrics, the method disclosed by the invention has small dependence on the type and structure of the modified base material, is suitable for the durable flame-retardant after-finishing modification of various fiber fabrics, and has certain universality.
Detailed Description
The invention provides a preparation method of durable flame-retardant after-finishing fabric, which comprises the following steps:
soaking the fabric in a photosensitive monomer finishing liquid, and performing first padding finishing to obtain a padded fabric;
carrying out a photo-grafting reaction on the padded fabric to obtain a photo-grafted modified fabric;
and soaking the photo-grafting modified fabric in a metal salt finishing solution, and performing second padding finishing to obtain the durable flame-retardant after-finishing fabric.
In the present invention, the starting materials or reagents required are commercially available products well known to those skilled in the art unless otherwise specified.
The method comprises the steps of soaking the fabric in photosensitive monomer finishing liquid, and carrying out first padding finishing to obtain the padded fabric. In the present invention, the fabric preferably includes cotton fabric, polyester fabric, nylon fabric, acryl fabric or polyacrylonitrile fabric. In the invention, the density of the fabric is preferably 105-122 g/m2The specific specification of the fabric is not particularly limited, and commercially available products with specifications well known in the art can be selected, and in the embodiment of the invention, the fabric with the size of 150mm × 58mm is specifically selected. Before the fabric is soaked in the photosensitive monomer finishing liquid, the invention preferably adopts 5 percent by mass of sodium carbonate aqueous solution to carry out boiling desizing treatment on the fabric, and then the fabric is dried for 1 hour at 80 ℃. The invention facilitates the finishing agent to be attached to the surface of the fabric through boiling desizing.
In the present invention, the photosensitive monomer finishing liquid preferably includes a photosensitive monomer, a photocrosslinking agent, a photoinitiator, and a solvent, the photosensitive monomer preferably includes acrylamide, methacrylamide, or acrylic acid; the photocrosslinking agent is N, N' -methylene bisacrylamide; the photoinitiator preferably comprises benzophenone, 1- [4- (2-hydroxyethoxy) -phenylene ] -2-hydroxy-2 ', 2' -dimethylethanone or 2-hydroxy-2-toluene-1-phenyl-1-propanone; the solvent is preferably deionized water or acetone.
In the invention, in the photosensitive monomer finishing liquid, the mass fraction of the photosensitive monomer is preferably 10-30%, more preferably 15-25%, and further preferably 20%; the mass fraction of the photocrosslinking agent is preferably 0.5-5.0%, more preferably 1.0-4.0%, and further preferably 2.0-3.0%; the mass fraction of the photoinitiator is preferably 0.5-3.0%, more preferably 1.0-2.5%, and even more preferably 1.5-2.0%. The invention utilizes the photocrosslinking agent to improve the grafting efficiency of the photosensitive monomer and graft photograft chains containing ligand groups to the surface of the fabric more.
The bath ratio of the fabric to the photosensitive monomer finishing liquid is not specially limited, and the amount of the photosensitive monomer finishing liquid can be used for completely soaking the fabric.
In the invention, the soaking time of the first padding finishing is preferably 20min to 1h, more preferably 30min to 50min, and further preferably 35min to 45 min; the rotation speed of the rolling mill is preferably 0.2m/s, and the pressure is preferably 0.5-1.0 MPa, more preferably 0.6-0.8 MPa.
In the first padding finishing process, the photosensitive monomer, the photoinitiator and the photocrosslinking agent in the photosensitive monomer finishing liquid are attached to the surface of the fabric.
After the first padding finishing is finished, the method preferably does not carry out any treatment, and the padded fabric is directly subjected to a photo-grafting reaction.
After the padded fabric is obtained, the padded fabric is subjected to a photo-grafting reaction to obtain the photo-grafted modified fabric. Preferably, the padded fabric is put into a photo-grafting box for photo-grafting reaction; the ultraviolet lamp intensity of the photografting reaction is preferably 100W/cm2(ii) a The irradiation time is preferably 15-40 min, more preferably 20-35 min, and further preferably 25-30 min; the irradiation height is preferably 5-30 cm, more preferably 10-25 cm, and further preferably 15-20 cm.
In the light grafting modification reaction process, the photosensitive monomer with the ligand group is covalently grafted on the surface of the fabric, so that the surface of the fabric is provided with the ligand group on the photosensitive monomer, such as an amide group, a carboxylic acid group and the like, and a light grafted chain with the ligand group is formed.
After the photo-grafting reaction is finished, the obtained fabric is preferably washed by using clear water, and then the obtained fabric is dried in an oven at the temperature of 80-100 ℃ for 30 min-1 h to obtain the photo-grafted modified fabric. The degree of rinsing with the clear water is not particularly limited in the present invention, and the residual monomers on the resulting fabric are washed clean or to a constant weight according to procedures well known in the art.
After the photo-grafted modified fabric is obtained, the photo-grafted modified fabric is soaked in a metal salt finishing liquid for second padding finishing to obtain the durable flame-retardant after-finishing fabric. In the present invention, the metal salt finishing liquid preferably includes a metal salt, a pH adjuster, and water; the metal salt preferably comprises a water-soluble calcium salt, zinc salt, aluminum salt, ferrous salt, ferric salt or copper salt; the pH adjuster preferably comprises sodium carbonate, hydrochloric acid or ammonium chloride; the water is preferably deionized water.
In the invention, the concentration of the metal salt in the metal salt finishing liquid is preferably 0.5-3.0 mol/L, more preferably 1.0-2.5 mol/L, and further preferably 1.5-2.0 mol/L; the concentration of the pH regulator is preferably 0.5-5 g/L, more preferably 1.0-4.0 g/L, and even more preferably 2.0-3.0 g/L.
The bath ratio of the photo-grafted modified fabric to the metal salt finishing liquid is not specially limited, and the metal salt finishing liquid can be used in an amount capable of completely infiltrating the photo-grafted modified fabric.
In the invention, the soaking time of the second padding finishing is preferably 20min to 1h, more preferably 30min to 50min, and further preferably 35min to 45 min; the rotation speed of the rolling mill is preferably 0.2 m/s; the pressure is preferably 0.5 to 1.0MPa, more preferably 0.6 to 0.8MPa, and still more preferably 0.65 to 0.75 MPa.
And in the second padding finishing process, carrying out coordination crosslinking on metal ions in the metal salt finishing liquid and ligand groups on the photograft chains.
The type of the rolling machine used for the first padding finishing and the second padding finishing is not specially limited, and the rolling machine with the type known in the field can be selected.
After the second padding finishing is finished, the obtained modified fabric is preferably dried in an oven at 80-100 ℃ for 30 min-1 h, then washed by clean water and dried in an oven at 100 ℃ for 30 min. The degree of washing is not particularly limited in the present invention, and the modified fabric may be washed clean according to procedures well known in the art.
The invention provides durable flame-retardant after-finishing fabric prepared by the preparation method in the technical scheme. In the preparation method of the invention, a photografting reaction covalently grafts a photosensitive monomer (such as acrylic acid, acrylamide and the like) containing ligand groups (such as amide groups, carboxylic acid groups and the like) on the surface of the fabric to obtain a modified fabric with the ligand groups, and then the modified fabric with the ligand groups is soaked in a metal salt solution, wherein the ligand groups can be coordinated with metal ions, and the metal ions are subjected to coordination crosslinking among the ligand groups on a photografted chain to obtain the durable flame-retardant afterfinish fabric. The durable flame-retardant after-finishing fabric prepared by the invention has the oxygen index of 36.8, has no molten drop phenomenon during combustion, can keep the oxygen index at about 29.0 after washing, and has durable flame retardance.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adopting 5 percent sodium carbonate aqueous solution by mass to nylon fabric (PA66, the fabric density is 122 g/m) with the size of 150mm multiplied by 58mm2) Boiling for desizing, drying for 1h at 80 ℃, soaking the obtained fabric in 500mL of photosensitive monomer finishing liquid, and performing first padding finishing, wherein in the photosensitive monomer finishing liquid, acetone is used as a solvent, the mass fraction of photosensitive monomer acrylamide is 30%, the mass fraction of photoinitiator benzophenone is 1.0%, the mass fraction of photocrosslinking agent N, N' -methylene bisacrylamide is 1.5%, the soaking time is 1h, the rotating speed of a rolling mill is 0.2m/s, and the pressure is 0.5MPa, so that the padded fabric is obtained;
placing the padded fabric into a photo-grafting box for photo-grafting reaction, wherein the intensity of an ultraviolet lamp is 100w/cm2The irradiation time is 40min, the irradiation height is 15cm, then the obtained fabric is washed by a large amount of clear water, and the washed fabric is placed into an oven at 100 ℃ for drying for 30min to obtain the photo-grafted modified fabric;
soaking the photo-grafted modified fabric in 500mL of metal salt finishing liquid for second padding finishing, wherein deionized water is used as a solvent, and metal salt FeCl is used as a metal salt2The concentration is 1.0mol/L, the concentration of ammonium chloride is 2.0gand/L, soaking for 1h, controlling the rotating speed of a rolling mill to be 0.2m/s and the pressure to be 0.5MPa, drying the obtained fabric in an oven at 80 ℃ for 50min, washing the fabric with clear water, and drying the washed fabric in an oven at 100 ℃ for 30min to obtain the after-finishing fabric.
The flame retardance test of the after-finishing fabric of the embodiment is carried out by adopting the method of national standard GB/T2403-1993, and the result shows that the after-finishing fabric has the Limiting Oxygen Index (LOI) of 36.8, is self-extinguished after leaving fire in vertical combustion, has the LOI of 28.3 after being washed for 10 times, and has better durable flame retardance.
Example 2
Adopting sodium carbonate aqueous solution with the mass fraction of 5 percent to the polyester fabric with the size of 150mm multiplied by 58mm (the fabric density is 105 g/m)2) Boiling for desizing, drying for 1h at 80 ℃, soaking the obtained fabric in 500mL of photosensitive monomer finishing liquid for first padding finishing, wherein in the photosensitive monomer finishing liquid, acetone is used as a solvent, the mass fraction of photosensitive monomer acrylic acid is 20%, and a photoinitiator 1- [4- (2-hydroxyethoxy) -phenylene]The mass fraction of the-2-hydroxy-2 ', 2 ' -dimethyl ethyl ketone is 3.0 percent, the mass fraction of the photocrosslinking agent N, N ' -methylene bisacrylamide is 5.0 percent, the soaking time is 20min, the rotating speed of a rolling mill is 0.2m/s, and the pressure is 1.0MPa, so that the padded fabric is obtained;
placing the padded fabric into a photo-grafting box for photo-grafting reaction, wherein the intensity of an ultraviolet lamp is 100w/cm2The irradiation time is 20min, the irradiation height is 30cm, then the obtained fabric is washed by a large amount of clear water, and the washed fabric is placed into an oven at 80 ℃ for drying for 40min to obtain the photo-grafted modified fabric;
soaking the photo-grafted modified fabric in 500mL of metal salt finishing liquid for second padding finishing, wherein deionized water is used as a solvent in the metal salt finishing liquid, and metal salt Al is used as a metal salt2(SO4)3The concentration is 3.0mol/L, the concentration of hydrochloric acid is 0.5g/L, the soaking time is 30min, the rotating speed of a rolling mill is 0.2m/s, the pressure is 1.0MPa, the obtained fabric is placed into a 100 ℃ oven to be dried for 30min, then the fabric is washed by clean water and then is placed into the 100 ℃ oven to be dried for 30min, and the after-finishing fabric is obtained.
The finished fabric of this example was tested for flame retardancy as in example 1 and showed a limiting oxygen index of 33.2, self-extinguishment from vertical burn without melt dripping, an LOI of 26.5 after 10 washes and a good durable flame retardancy.
Comparative example 1
Adopting 5 percent sodium carbonate aqueous solution by mass to nylon fabric (PA66, the fabric density is 122 g/m) with the size of 150mm multiplied by 58mm2) Boiling for desizing, drying for 1h at 80 ℃, soaking the obtained fabric in 500mL of photosensitive monomer finishing liquid, and performing first padding finishing, wherein in the photosensitive monomer finishing liquid, acetone is used as a solvent, the mass fraction of photosensitive monomer acrylamide is 30%, the mass fraction of photoinitiator benzophenone is 1.0%, the mass fraction of photocrosslinking agent N, N' -methylene bisacrylamide is 1.5%, the soaking time is 1h, the rotating speed of a rolling mill is 0.2m/s, and the pressure is 0.5MPa, so that the padded fabric is obtained;
placing the padded fabric into a photo-grafting box for photo-grafting reaction, wherein the intensity of an ultraviolet lamp is 100w/cm2The irradiation time is 40min, the irradiation height is 15cm, then the obtained fabric is washed by a large amount of clear water, and the washed fabric is placed into an oven at 100 ℃ for drying for 30min to obtain the after-finishing fabric.
The flame retardancy test of the finished fabric of this comparative example was conducted in accordance with the procedure of example 1, and the results showed that the prepared finished fabric had a limiting oxygen index of 25.6, complete destruction by vertical burning, an LOI of 23.0 after 10 washes, and poor durable flame retardancy.
Comparative example 2
Adopting 5 percent sodium carbonate aqueous solution by mass to nylon fabric (PA66, the fabric density is 122 g/m) with the size of 150mm multiplied by 58mm2) Boiling for desizing, drying for 1h at 80 ℃, putting the obtained fabric into 500mL of metal salt finishing liquid for padding finishing, wherein deionized water is used as a solvent, and metal salt FeCl is used as a metal salt finishing liquid2The concentration is 1.0mol/L, the concentration of ammonium chloride is 2.0g/L, the soaking time is 1h, the rotation speed of a rolling mill is 0.2m/s, the pressure is 0.5MPa, the obtained fabric is put into an oven at 80 ℃ for drying for 50min, and then the fabric is washed by clean water and then is put into a roomAnd drying in an oven at 100 ℃ for 30min to obtain the after-finishing fabric.
The finished fabric of this comparative example was tested for flame retardancy as in example 1 and showed a limiting oxygen index of 32.8 for the finished fabric prepared, self-extinguishing from fire in vertical burn, and after 10 washes, an LOI of 20.3 with no durable flame retardancy.
According to examples 1-2 and comparative examples 1-2, the flame retardant durability of the post-treated fabric obtained by single photo-grafting modification and metal salt modification is poor or no durable flame retardant property, while the post-treated fabric prepared by the photo-grafting modification process combined with metal salt coordination reaction in examples 1-2 of the invention has excellent durable flame retardant property.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of durable flame-retardant after-finishing fabric is characterized by comprising the following steps:
soaking the fabric in a photosensitive monomer finishing liquid, and performing first padding finishing to obtain a padded fabric;
carrying out a photo-grafting reaction on the padded fabric to obtain a photo-grafted modified fabric;
and soaking the photo-grafting modified fabric in a metal salt finishing solution, and performing second padding finishing to obtain the durable flame-retardant after-finishing fabric.
2. The method of claim 1, wherein the fabric comprises cotton fabric, polyester fabric, nylon fabric, acryl fabric, or polyacrylonitrile fabric.
3. The preparation method according to claim 1, wherein the photosensitive monomer finishing liquid comprises a photosensitive monomer, a photocrosslinking agent, a photoinitiator and a solvent, wherein the photosensitive monomer comprises acrylamide, methacrylamide or acrylic acid; the photocrosslinking agent is N, N' -methylene bisacrylamide; the photoinitiator comprises benzophenone, 1- [4- (2-hydroxyethoxy) -phenylene ] -2-hydroxy-2 ', 2' -dimethyl ethyl ketone or 2-hydroxy-2-toluene-1-phenyl-1-acetone; the solvent is deionized water or acetone.
4. The preparation method according to claim 3, wherein in the photosensitive monomer finishing liquid, the mass fraction of the photosensitive monomer is 10-30%, and the mass fraction of the photocrosslinking agent is 0.5-5.0%; the mass fraction of the photoinitiator is 0.5-3.0%.
5. The preparation method according to claim 1, wherein the soaking time of the first padding finishing is 20min to 1h, the rotation speed of a rolling mill is 0.2m/s, and the pressure is 0.5 to 1.0 MPa.
6. The method of claim 1, wherein the UV lamp intensity of the photografting reaction is 100W/cm2The irradiation time is 15-40 min, and the irradiation height is 5-30 cm.
7. The production method according to claim 1, wherein the metal salt finishing liquid comprises a metal salt, a pH adjuster, and water; the metal salt comprises water-soluble calcium salt, zinc salt, aluminum salt, ferrous salt, ferric salt or copper salt; the pH regulator comprises sodium carbonate, hydrochloric acid or ammonium chloride.
8. The preparation method according to claim 7, wherein the concentration of the metal salt in the metal salt finishing liquid is 0.5-3.0 mol/L, and the concentration of the pH regulator is 0.5-5 g/L.
9. The preparation method according to claim 1, wherein the soaking time of the second padding finishing is 20min to 1h, the rotation speed of a rolling mill is 0.2m/s, and the pressure is 0.5 to 1.0 MPa.
10. The durable flame-retardant after-finishing fabric prepared by the preparation method of any one of claims 1 to 9.
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