CN114657779A - Durable intumescent flame-retardant protein fiber product and preparation method thereof - Google Patents

Durable intumescent flame-retardant protein fiber product and preparation method thereof Download PDF

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CN114657779A
CN114657779A CN202210356622.2A CN202210356622A CN114657779A CN 114657779 A CN114657779 A CN 114657779A CN 202210356622 A CN202210356622 A CN 202210356622A CN 114657779 A CN114657779 A CN 114657779A
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protein fiber
fiber product
durable
flame retardant
terephthalaldehyde
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CN114657779B (en
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程献伟
顾靓
关晋平
陈国强
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Suzhou University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating 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
    • D06M13/282Treating 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
    • D06M13/292Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/12Aldehydes; Ketones
    • D06M13/127Mono-aldehydes, e.g. formaldehyde; Monoketones
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/61Polyamines polyimines
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • D06M2101/12Keratin fibres or silk
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a durable intumescent flame retardant protein fiber product and a preparation method thereof, and relates to the technical field of textile finishing. The invention takes phytic acid, terephthalaldehyde and polyeneimine as raw materials to construct an expansion flame-retardant coating on the surface of a protein fiber product, firstly the phytic acid and the terephthalaldehyde are respectively introduced onto the protein fiber product through ionic bonds and covalent bonds, and then the polyeneimine and the terephthalaldehyde on the protein fiber product are subjected to Schiff base reaction to form a high-adhesion insoluble coating on the surface of the protein fiber. The coating is crosslinked on the surface of a protein fiber product through covalent bonds, is insoluble in water, has high adhesiveness to protein fibers, and can effectively prevent phytic acid from diffusing to the outside of the fibers. Therefore, the protein fiber product has high flame retardant efficiency, excellent water washing resistance, wide application prospect and important practical application value.

Description

Durable intumescent flame-retardant protein fiber product and preparation method thereof
Technical Field
The invention relates to the technical field of textile finishing, in particular to a durable intumescent flame retardant protein fiber product and a preparation method thereof.
Background
The protein fiber has the characteristics of special heat retention, soft luster, comfortable wearing and the like. With the improvement of the living standard of people and the transformation of consumption concept, people are pursuing products made of natural textile raw materials, and high-grade products of protein fibers are widely applied to the textile industry. However, the protein fiber cannot be self-extinguished after being ignited for continuous combustion, and the flame retardant property of the protein fiber needs to be further improved.
In recent years, with the improvement of environmental protection call and the improvement of sustainable development requirements, the development of flame retardants and flame retardant technologies is developing towards the direction of non-toxicity, harmlessness, environmental friendliness and resource conservation. The biomass material has a series of characteristics of being green, harmless, renewable, degradable and the like, can replace chemical reagents which are harmful to organisms and are not easy to decompose, and plays a role in the field of flame-retardant materials. The phytic acid has high phosphorus content and high flame retardant efficiency, and has been paid attention to the field of flame retardance of textiles. The document (ChengXW, guanJP, ChenG, YangXH, TangRC, adsorbed flame retardant textile of bio-based flame retardant fibers [ J ]. Polymers, 2016, 8 (4): 122) uses phytic acid to improve the flame retardant performance of wool fabrics by electrostatic attraction adsorption, but phytic acid has good water solubility and diffuses to the outside of the fibers during water washing, resulting in poor water washing resistance of the flame retardant wool fabrics.
In the literature (Liu Xin Hua, Liu Hai Long, Fang Yin Chun, Yan Peng, Hou guang, preparation of polyethylene imine/phytic acid layer-by-layer self-assembly flame-retardant polyester/cotton blended fabric and performance thereof [ J ]. textile science and report, 2021, 42 (11): 103-109), polyethylene imine and phytic acid are used as raw materials, a flame-retardant coating is constructed on the surface of the polyester/cotton blended fabric to improve the flame-retardant performance of the polyester/cotton blended fabric, but the ionic bond between the phytic acid and the polyethylene imine is unstable, so that the coating is not resistant to water washing; therefore, the phytic acid and the polyethyleneimine solution are repeatedly dipped on the surface of the polyester/cotton blended fabric for multiple times by adopting a layer-by-layer self-assembly method, so that the water washing resistance of the flame-retardant coating is improved, but the method has the defects of complex flow, long time consumption and limited improvement degree of the water washing resistance of the flame-retardant coating.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the problems of complicated preparation process, long time consumption and poor water washing resistance of the phytic acid flame-retardant protein fiber product in the prior art.
In order to solve the technical problems, the invention provides a durable intumescent flame retardant protein fiber product and a preparation method thereof. The invention takes phytic acid, terephthalaldehyde and polyeneimine as raw materials to construct an expansion flame-retardant coating on the surface of a protein fiber product, firstly, the phytic acid and the terephthalaldehyde are respectively combined with protein fibers through ionic bonds and covalent bonds, and then the polyeneimine and the terephthalaldehyde on the protein fiber product are subjected to Schiff base reaction to form a high-adhesion insoluble coating on the surface of the protein fibers. The coating is crosslinked on the surface of the protein fiber through covalent bonds, is insoluble in water, has high adhesiveness to the protein fiber, and can effectively prevent phytic acid from diffusing to the outside of the fiber to prepare the durable intumescent flame retardant protein fiber product.
The first object of the present invention is to provide a method for preparing a durable intumescent flame retardant protein fiber product, comprising the steps of:
(1) dissolving phytic acid and terephthalaldehyde in an alcohol solution to obtain a finishing solution, and immersing the protein fiber product into the finishing solution for heating to obtain a finished protein fiber product;
(2) and (2) immersing the finished protein fiber product in the step (1) into a poly (alkylenimine) solution for heating to obtain the durable intumescent flame retardant protein fiber product.
In one embodiment of the present invention, in the step (1), the concentration of phytic acid in the finishing liquor is 40-120g/L, and the concentration of terephthalaldehyde is 40-80 g/L; the mass volume ratio of the terephthalaldehyde to the alcohol is 1 g: 4-5 mL. The phytic acid has high concentration and good flame retardant effect, but is wasted if the concentration is too high; the terephthalaldehyde is combined with the polyeneimine, the dosage of the terephthalaldehyde is high, the coating effect of the terephthalaldehyde and the polyeneimine formed on the protein fiber fabric is good, but if the dosage of the terephthalaldehyde and the polyeneimine is too high, the coating is too thick, waste is caused, and the damage to the hand feeling of the protein fiber fabric is serious; the dosage of the alcohol in the invention can ensure that the terephthalaldehyde is better dissolved in the alcohol solution, and the excessive dosage is wasted.
In one embodiment of the present invention, in the step (1), the heating temperature is 80-90 ℃ and the heating time is 30-60 min. In the temperature and time range, the phytic acid and the terephthalaldehyde can well react with protein fibers.
In one embodiment of the invention, in the step (1), the mass ratio of the protein fiber product to the finishing liquor is 1: 20-50. If the mass ratio of the protein fiber product to the finishing liquid is too low, the finished protein fiber is not uniform, and if the mass ratio of the protein fiber product to the finishing liquid is too high, the protein fiber is wasted.
In one embodiment of the present invention, in step (1), the solvent of the alcohol solution is ethanol.
In one embodiment of the present invention, in the step (2), the polyalkyleneimine is polypropyleneimine and/or polyethyleneiminine.
In one embodiment of the present invention, in step (2), the concentration of the polyalkyleneimine in the polyalkyleneimine solution is from 30 to 50 g/L.
In one embodiment of the present invention, in the step (2), the heating temperature is 60-70 ℃ and the heating time is 20-40 min. Within the temperature and time provided by the invention, covalent bond bonding can be better generated between the terephthalaldehyde and the polyacrylamide, ionic bond bonding can be better generated between the phytic acid and the polyeneimine, and the terephthalaldehyde and the polyacrylamide are deposited on the surface of the protein fiber fabric, and the terephthalaldehyde is wasted if the temperature is too high or the time is too long.
In one embodiment of the invention, in step (2), the mass ratio of the finished protein fiber product to the polyalkyleneimine solution is 1: 20-50.
In one embodiment of the invention, the protein fiber product is wool fiber or fabric, silk fiber or fabric.
The second purpose of the invention is to provide a durable intumescent flame retardant protein fiber product prepared by the method.
The principle of the invention is as follows: the phytic acid is mainly combined with protein fibers by means of ionic bonds, so that the washing resistance is poor; the terephthalaldehyde and the protein fiber product can be combined by covalent bonds generated by Schiff base, and redundant aldehyde groups of the terephthalaldehyde and amino groups of the polyalkyleneimine are subjected to Schiff base reaction to generate high-adhesion insoluble precipitates to cover the surface of the protein fiber. In the washing process, redundant amino groups of the polyeneimine can be combined with phytic acid through ionic bonds, so that the phytic acid is retained on the protein fiber, the water solubility of the coating is reduced, and the washing resistance of the coated protein fiber product is improved. In addition, phytic acid is used as an acid source, polyethyleneimine is used as a gas source, and terephthalaldehyde is used as a char forming agent to form an intumescent flame retardant system, during the thermal cracking process, the intumescent flame retardant coating can be decomposed to generate phosphorus-containing flame retardant groups, non-combustible nitrogen-containing gas and the like, an intumescent char layer is rapidly formed on the surface of protein fibers, and a protective layer is formed on the surface of the fibers to isolate heat and oxygen, so that the flame retardant property of the protein fiber product is improved.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the durable intumescent flame-retardant protein fiber product disclosed by the invention forms a flame-retardant coating in the preparation process, and the flame-retardant coating has the advantages of high phosphorus content, high nitrogen content, strong foaming and carbonizing capabilities, high flame-retardant efficiency and capability of effectively improving the flame-retardant property of the protein fiber product. In addition, the expanded coating has high adhesion capacity by virtue of covalent bond combination between terephthalaldehyde and polyacrylamide and ionic bond combination between phytic acid and polyeneimine, is coated on the surface of the protein fiber through covalent bonds, is high in bonding firmness, and can effectively inhibit the phytic acid flame retardant from diffusing to the outside of the fiber, so that the flame-retardant protein fiber product has high water washing resistance.
(2) The preparation method provided by the invention is simple and convenient in process, mild in reaction conditions, and wide in application prospect and important in practical application value.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which:
fig. 1 is an apparent topography of the flame-retardant silk double-crepe fabric in example 1 of the invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
A durable intumescent flame retardant silk crepe fabric and a preparation method thereof comprise the following specific steps:
(1) dissolving phytic acid and terephthalaldehyde in a mixed solution of distilled water and ethanol to obtain a finishing solution, wherein the concentration of the phytic acid is 100g/L, the concentration of the terephthalaldehyde is 50g/L, and the mass volume ratio of the terephthalaldehyde to the ethanol is 1 g: 5mL, putting the silk crepe fabric into finishing liquid, heating to 85 ℃, and then preserving heat for 50min to obtain finished silk crepe; the mass ratio of the silk double-crepe fabric to the finishing liquid is 1: 50.
(2) immersing the finished silk crepe-de-chine fabric into a polypropylene imine solution, wherein the concentration of the polypropylene imine is 45g/L, and the mass ratio of the finished silk crepe-de-chine fabric to the polypropylene imine solution is 1: and 50, heating to 65 ℃, and then preserving the heat for 30min to obtain the durable intumescent flame retardant silk crepe fabric.
Comparative example 1
The method is basically the same as example 1, except that no terephthalaldehyde and no polypropyleneimine are added in steps (1) and (2), respectively, i.e., the flame-retardant system only contains phytic acid and does not contain terephthalaldehyde and polypropyleneimine.
Example 2
A durable intumescent flame retardant silk electric power textile fabric and a preparation method thereof comprise the following specific steps:
(1) dissolving phytic acid and terephthalaldehyde into a mixed solution of distilled water and ethanol to obtain a finishing liquid, wherein the concentration of the phytic acid is 120g/L, the concentration of the terephthalaldehyde is 80g/L, and the mass-volume ratio of the terephthalaldehyde to the ethanol is 1 g: 4mL, putting the silk electric textile into finishing liquid, heating to 80 ℃, and keeping the temperature for 60min to obtain finished silk electric textile; the mass ratio of the silk electric power textile fabric to the finishing liquid is 1: 20.
(2) the finishing silk electric power textile fabric is immersed in a polypropylene imine solution, the concentration of the polypropylene imine is 50g/L, and the mass ratio of the finishing silk electric power textile fabric to the polypropylene imine solution is 1: and 20, heating to 60 ℃, and preserving heat for 40min to obtain the durable intumescent flame-retardant silk electric power textile fabric.
Example 3
A durable intumescent flame-retardant wool fabric and a preparation method thereof comprise the following steps:
(1) dissolving phytic acid and terephthalaldehyde into a mixed solution of distilled water and ethanol to obtain a finishing liquid, wherein the concentration of the phytic acid is 40g/L, the concentration of the terephthalaldehyde is 40g/L, and the mass-to-volume ratio of the terephthalaldehyde to the ethanol is 1 g: 4.5mL, putting the wool fabric into finishing liquid, heating to 90 ℃, and then preserving heat for 50min to obtain a finished wool fabric; the mass ratio of the wool fabric to the finishing liquid is 1: 40.
(2) soaking the finished wool fabric into a polypropylene imine solution, wherein the concentration of polypropylene imine is 30g/L, and the mass ratio of the finished wool fabric to the polypropylene imine solution is 1: and 40, heating to 70 ℃, and then preserving the heat for 35min to obtain the durable intumescent flame-retardant wool fabric.
Example 4
A durable intumescent flame-retardant wool fabric and a preparation method thereof comprise the following steps:
(1) dissolving phytic acid and terephthalaldehyde into a mixed solution of distilled water and ethanol to obtain a finishing liquid, wherein the concentration of the phytic acid is 80g/L, the concentration of the terephthalaldehyde is 60g/L, and the mass-to-volume ratio of the terephthalaldehyde to the ethanol is 1 g: 4.5mL, putting the wool fabric into finishing liquid, heating to 85 ℃, and then preserving heat for 50min to obtain a finished wool fabric; the mass ratio of the wool fabric to the finishing liquid is 1: 35.
(2) soaking the finished wool fabric into a polypropylene imine solution, wherein the concentration of polypropylene imine is 40g/L, and the mass ratio of the finished wool fabric to the polypropylene imine solution is 1: and 35, heating to 67 ℃, and keeping the temperature for 30min to obtain the durable intumescent flame-retardant wool fabric.
Comparative example 2
The method is basically the same as example 4, except that no phytic acid is added in the step (1), namely the flame-retardant system only contains terephthalaldehyde and polypropylene imine.
Comparative example 3
The method is basically the same as example 4, except that no terephthalaldehyde is added in the step (1), namely, the flame-retardant system only contains phytic acid and polypropyleneimine.
Test example 1
The durable intumescent flame retardant silk double-crepe fabric of example 1 was characterized, and as shown in fig. 1, it was observed from the scanning electron microscope picture that the surface of the finished fabric was covered with a uniform coating layer, which is a precipitate generated by the covalent bonding of terephthalaldehyde and polyalkyleneimine, and such a coating layer was firmly adhered to the surface of the fabric through the covalent bonding, thereby imparting durable flame retardant property to the flame retardant fabric.
Test example 2
The flame retardant and water washing resistance of the durable intumescent flame retardant silk double-creped fabric of example 1, the silk double-creped fabric of comparative example 1, the durable intumescent flame retardant silk electrical textile fabric of example 2, the durable intumescent flame retardant wool fabrics of examples 3-4, and the wool fabric of comparative example 2 were tested.
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 burning performance.
The combustion performance of the fabric is evaluated according to the GB/T17591-2006 flame-retardant fabric standard.
The washing method is described in AATCC61-2006 accelerated test of the fastness to washing for domestic and commercial purposes.
Table 1 shows the final measured flame retardant and water wash resistance of the flame retardant silk and wool fabrics:
TABLE 1 flame retardancy and Water washing resistance of Silk and wool fabrics
Figure BDA0003583273390000071
As can be seen from Table 1, the unfinished silk and wool fabrics completely burned in the vertical burning process, and the damaged length was 30cm after washing 0 times and 20 times, indicating that the flame retardant property was poor. The damage length of the silk and wool fabrics after flame-retardant finishing by the intumescent coating is obviously reduced, and the damage length is less than 15cm after 0 time and 20 times of water washing, so that the damage length reaches B in GB/T17591-2006 flame-retardant fabrics1The requirement of grade flame retardant performance shows that the water washing resistance of the flame retardant silk and wool products is excellent. The results show that the silk and wool products finished by the method have good flame retardant property and water washing resistance.
Comparing example 1 with comparative example 1 and comparing example 4 with comparative examples 2-3, it can be seen that the flame retardant performance of the silk fabric is better after the phytic acid is independently finished, but the silk fabric is completely burnt after being washed for 20 times and loses the flame retardant effect, which indicates that the water washing resistance of the phytic acid finished silk fabric is poor because no sticky precipitate is deposited on the surface of the silk fabric. The wool fabric finished by the terephthalaldehyde and the polypropylene imine is completely combusted before and after being washed by water, which shows that the flame retardant property of the wool fabric is poor. The wool fabric finished by the phytic acid and the polyethyleneimine has higher flame retardant effect, but loses the flame retardant effect after being washed for 10 times, which shows that the washing resistance of the finished wool fabric is poor because no sticky precipitate is deposited on the surface of the wool fabric.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.

Claims (10)

1. A method for preparing a durable intumescent flame retardant protein fiber product is characterized by comprising the following steps,
(1) dissolving phytic acid and terephthalaldehyde in an alcohol solution to obtain a finishing solution, and immersing the protein fiber product into the finishing solution for heating to obtain a finished protein fiber product;
(2) and (2) immersing the finished protein fiber product in the step (1) into a poly (alkylenimine) solution for heating to obtain the durable intumescent flame retardant protein fiber product.
2. The method for preparing a durable intumescent flame retardant protein fiber product according to claim 1, wherein in step (1), the concentration of phytic acid in the finishing liquor is 40 to 120g/L, and the concentration of terephthalaldehyde is 40 to 80 g/L; the mass volume ratio of the terephthalaldehyde to the alcohol is 1 g: 4-5 mL.
3. The method for preparing a durable intumescent flame retardant protein fiber product according to claim 1, wherein in step (1), the heating temperature is 80-90 ℃ and the heating time is 30-60 min.
4. The method for preparing a durable intumescent flame retardant protein fiber product according to claim 1, wherein in the step (1), the mass ratio of the protein fiber product to the finishing liquor is 1: 20-50.
5. The method for preparing a durable intumescent flame retardant protein fiber product according to claim 1, wherein in step (2), the polyalkyleneimine is polypropyleneimine and/or polyethyleneiminine.
6. The method for preparing a durable intumescent flame retardant protein fiber product as claimed in claim 1, wherein in step (2), the concentration of the polyeneimine in the polyeneimine solution is 30-50 g/L.
7. The method for preparing a durable intumescent flame retardant protein fiber product according to claim 1, wherein in step (2), the heating temperature is 60-70 ℃ and the heating time is 20-40 min.
8. The method for preparing a durable intumescent flame retardant protein fiber product as claimed in claim 1, wherein in step (2), the mass ratio of the finished protein fiber product to the polyalkyleneimine solution is 1: 20-50.
9. The method of claim 1 wherein the protein fiber product is wool fiber or fabric, silk fiber or fabric.
10. A durable intumescent flame retardant protein fibre product prepared by the process of any of claims 1 to 9.
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CN117188148A (en) * 2023-11-06 2023-12-08 江苏恒力化纤股份有限公司 Layer-by-layer assembly preparation method of durable flame-retardant coating polyester/cotton blended fabric

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XIAN-WEI CHENG 等: ""Flame retardant coating of wool fabric with phytic acid_polyethyleneimine polyelectrolyte complex"", 《PROGRESS IN ORGANIC COATINGS》 *
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116516679A (en) * 2023-03-30 2023-08-01 苏州大学 Durable flame-retardant anti-dripping coating nylon 6 fabric and preparation method thereof
CN117188148A (en) * 2023-11-06 2023-12-08 江苏恒力化纤股份有限公司 Layer-by-layer assembly preparation method of durable flame-retardant coating polyester/cotton blended fabric
CN117188148B (en) * 2023-11-06 2024-03-19 江苏恒力化纤股份有限公司 Layer-by-layer assembly preparation method of durable flame-retardant coating polyester/cotton blended fabric

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