A high-efficiency flame-retardant fabric based on phytated nanocellulose fibers and a preparation method thereof

By covalently grafting phytic acid onto nanocellulose fibers and adsorbing with the fiber surface through covalent bonds, the problem of mechanical properties degraded by phytic acid penetration into the fibers is solved, achieving both high-efficiency flame retardant and mechanical properties.

CN119221285BActive Publication Date: 2025-05-13ZHEJIANG SCI-TECH UNIV +1
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Patent Information

Application Number
CN202411765069.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-04
Publication Date
2025-05-13
Estimated Expiration
2044-12-04

AI Technical Summary

Technical Problem

In the prior art, phytic acid penetrates into the fibers when used as a fabric flame retardant, resulting in polymer degradation in the fibers and significantly reduced mechanical properties. There is no public report on the use of phytic acid as a fabric flame retardant alone.

Method used

Phytic acid is covalently grafted onto nanocellulose fibers through the esterification reaction to form phytic acid esterified nanocellulose fibers, and chemically adsorbed with cotton fibers or polyester fibers treated with organic amines through covalent bonds to build a porous network structure layer to achieve flame retardant effect.

Benefits of technology

It effectively inhibits the degradation of polymers in the fibers, maintains the mechanical properties of the fabric, and at the same time imparts the fabrics with efficient flame retardant and durable properties, and retains the breathability, softness and hygroscopicity of the original fabric.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a highly efficient flame-retardant fabric based on phytated nanocellulose fibers and a preparation method thereof. Phytated nanocellulose fibers are attached to the fiber surface through chemical bonds, interlaced with each other to form a stacked porous network, and constitute a flame-retardant layer. The flame-retardant fabric is treated by impregnating the fabric with a dispersion of phytated cellulose fibers, and the phytated nanocellulose fibers are heated and baked to cause a chemical reaction between the phytated nanocellulose fibers and the fabric fibers to form covalent bonds. Since the phytated nanocellulose fibers are not easy to penetrate into the fiber core, the degradation of polymers in the fiber caused by phytic acid can be avoided, thereby effectively ensuring the mechanical properties of the fabric. The present invention uses bio-based raw materials, is green and environmentally friendly, and conforms to the concept of sustainable development.
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Description

Technical Field

[0001] The invention belongs to the field of preparation of new textile materials, and particularly relates to a high-efficiency flame-retardant fabric based on phytated nanocellulose fibers and a preparation method thereof. Background Art

[0002] Cotton, polyester and other fabrics are widely used in home decoration and clothing, especially cotton fabrics are more popular due to their unique characteristics of moisture absorption, breathability, softness and hygiene. However, cotton and polyester fabrics are flammable. Once they encounter fire, they will seriously threaten people's life safety and may cause huge property losses. Therefore, the development of flame-retardant fabrics is of great significance and application value.

[0003] The flame retardant function of fabrics is mainly achieved through post-finishing. Currently, the flame retardant post-finishing agents on the market can be divided into three categories: halogen, nitrogen and phosphorus. Among them, halogen flame retardants produce a large amount of toxic gases when burned. Nitrogen flame retardants are easy to decompose under high temperature conditions, which reduces their flame retardant properties and performs poorly in high temperature environments. In contrast, phosphorus flame retardants have the advantages of high efficiency, smokeless, low toxicity and no pollution, and have good development prospects.

[0004] Phytic acid (PA) can be extracted from plants. It has been widely used as a flame retardant in recent years because of its good biocompatibility, environmental friendliness, renewability and degradability, and rich in phosphorus. For example, Chinese invention patent CN110524657A uses phytic acid to treat wood samples, and uses the catalytic effect of phytic acid at high temperature to induce the formation of a dense protective carbon layer to achieve an efficient flame retardant effect; Chinese invention patent CN108314951A uses a layer-by-layer self-assembly method to construct a melamine-phytic acid flame retardant layer on the surface of molybdenum diselenide (MoSe2) nanosheets. The resulting molybdenum diselenide nanosheets are filled into epoxy resin to produce an efficient fireproof effect. However, phytic acid is strongly acidic. When used as a fabric flame retardant, it will penetrate into the fiber and induce the degradation of polymers in the fiber, resulting in a significant decrease in the mechanical properties of the fabric. Therefore, the application of phytic acid in the field of functional finishing of fabrics is limited, and there has been no public report on the use of phytic acid alone as a fabric flame retardant. Chinese invention patent CN115772235A discloses a method for synthesizing polyvinyl alcohol phytate, but when used as a flame retardant in fabrics, it cannot prevent the phytic acid component from penetrating into the interior of the fiber. Summary of the invention

[0005] In order to solve the problem of phytic acid inducing polymer degradation in fabric fibers in the prior art, the present invention provides a method for limiting the penetration of phytic acid molecules into the fiber core to ensure that the phytic acid components are only attached to the fiber surface, thereby inhibiting the reduction of the mechanical strength of the fabric and at the same time giving the fabric high-efficiency flame retardant properties. The specific technical scheme is as follows:

[0006] A highly effective flame-retardant fabric based on phytated nanocellulose fibers, wherein the phosphorus content of the phytated nanocellulose fibers is 4-6%, and the fabric is characterized in that the phytated nanocellulose fibers are attached to the surface of the fabric fibers through covalent bonds to form a porous network structure layer, and the porous network structure layer constitutes a flame-retardant layer. The phytated nanocellulose fibers are adsorbed on the fiber surface through covalent bonds, giving the fabric excellent flame-retardant and wash-resistant properties. At the same time, the mechanical properties, softness, and air permeability of the modified fabric are not significantly deteriorated, and the moisture absorption rate is significantly improved.

[0007] A method for preparing a highly effective flame-retardant fabric based on phytated nanocellulose fibers, wherein the fabric is a cotton fabric, comprises the following steps:

[0008] Step 1: dispersing the nanocellulose fibers in water, adding a phytic acid solution, heating for reaction, and washing away unreacted phytic acid small molecules after the reaction to obtain phytated nanocellulose fibers;

[0009] Step 2: dispersing the phytated nanocellulose fibers in deionized water to prepare a dispersion, immersing cotton fabric in the dispersion, controlling the wet weight after taking it out, heating and reacting under hot pressure, washing away the ungrafted phytated nanocellulose fibers, and drying to obtain a flame-retardant cotton fabric.

[0010] First, phytic acid is covalently grafted onto nanocellulose fibers through an esterification reaction to obtain phytated nanocellulose fibers. The phosphoric acid groups on the phytated nanocellulose fibers further undergo an esterification reaction with the hydroxyl groups on the surface of the cotton fibers to achieve chemical adsorption of a large amount of phytic acid components on the surface of the cotton fibers. Phytated nanocellulose fibers act as flame retardants to impart flame retardant properties to fabrics.

[0011] Furthermore, in step 1, the mass fraction of the solution after the nanocellulose fibers are dispersed is 2-3%, the mass fraction of the phytic acid solution is 4-6%, the reaction temperature is 80-100° C., and the reaction time is 4-5 hours.

[0012] Furthermore, in step 2, the mass fraction of the dispersion is 4-6%, the immersion treatment time is 2-3 minutes, the wet weight is controlled to be 170-200%, the reaction temperature is 170-200° C., and the time is 2-7 minutes.

[0013] A method for preparing a highly effective flame-retardant fabric based on phytated nanocellulose fibers, wherein the fabric is a polyester fabric. The method comprises the following steps:

[0014] Step 1: using an organic amine solution to modify polyester fabric to obtain aminated polyester;

[0015] Step 2: dispersing the nanocellulose fibers in water, adding phytic acid solution, heating for reaction, and washing away unreacted phytic acid small molecules after the reaction to obtain phytated nanocellulose fibers;

[0016] Step 3: dispersing the phytated nanocellulose fibers in deionized water to prepare a dispersion, immersing the aminated polyester in the dispersion, controlling the wet weight after taking it out, heating and reacting under hot pressure, washing away the ungrafted phytated nanocellulose fibers, and drying to obtain a flame-retardant polyester fabric.

[0017] Firstly, the polyester fabric is modified by atomizing an organic amine solution, and then the phytated nanocellulose fibers are grafted onto the fiber surface through an amidation reaction to impart flame retardancy to the fiber.

[0018] Furthermore, the organic amine solution in step 1 is an aminopropyltriethoxysilane solution, the mass fraction of the solution is 2-4%, the polyester fabric is immersed in it, the immersion time is 2-3 minutes, the wet weight is controlled to be 140-160%, the temperature is raised to 70-90° C., and the reaction is carried out for 5-10 minutes.

[0019] Furthermore, in step 2, the mass fraction of the solution after the nanocellulose fibers are dispersed is 2-3%, the mass fraction of the phytic acid solution is 4-6%, the reaction temperature is 80-100° C., and the reaction time is 4-5 hours.

[0020] Furthermore, in step three, the mass fraction of the dispersion is 4-6%, the immersion treatment time is 2-3 minutes, the wet weight is controlled to be 170-200%, the reaction temperature is 170-200° C., and the time is 2-7 minutes.

[0021] Experimental data show that as the concentration of phytic acid increases, the resulting phytated nanocellulose fibers can improve the flame retardant properties of cotton fabrics; when the concentration exceeds 6%, the mechanical properties of the fabric decrease.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] (1) The present invention synthesizes phytic acid-esterified nanocellulose fibers and uses them as a high-efficiency flame retardant to connect to the surface of fabric fibers through covalent bonds. While giving the fabric excellent flame retardant properties, it overcomes the adverse effects of the strong acidity of phytic acid on the chemical structure of the fibers and effectively maintains the mechanical properties of the fabric.

[0024] (2) The phytic acid and nanocellulose fibers used in the present invention are both bio-based raw materials, green and environmentally friendly, and in line with the concept of sustainable development.

[0025] (3) The flame retardant of the present invention is connected to the fabric through a covalent bond, so that the flame retardant fabric has excellent durability.

[0026] (4) The flame-retardant fabric of the present invention can retain the good air permeability, softness and hygroscopicity of the original cotton fabric. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 The flame retardant cotton fabric preparation process flow chart of the present invention;

[0028] Figure 2 The flame retardant polyester fabric preparation process flow chart of the present invention;

[0029] Figure 3 This is a vertical combustion comparison diagram of the flame-retardant cotton fabric prepared in Example 1 and the original cotton fabric;

[0030] Figure 4 This is a comparison chart of the softness of the flame-retardant cotton fabric prepared in Example 1 and the original fabric;

[0031] Figure 5 XRD comparison diagram of the flame retardant cotton fabric prepared in Example 1 and the original cotton fabric;

[0032] Figure 6 This is a SEM comparison picture of the flame-retardant cotton fiber prepared in Example 1 and the original cotton fiber. DETAILED DESCRIPTION

[0033] The technical solution of the present invention is further described below in conjunction with specific comparative examples and embodiments.

[0034] The high-efficiency flame-retardant fabric based on phytated nanocellulose fibers of the present invention uses nanocellulose fibers (CNF) as carriers, and after phytic acid (PA) is adsorbed through covalent bonds, it is loaded onto the surface of the fabric fibers to construct a high-efficiency flame-retardant layer. The diameter of the nanocellulose fibers is 1 to 20 nanometers. Phytic acid reacts with nanocellulose molecules to obtain phytated nanocellulose fibers (PA-CNF), and the phosphorus content is 4 to 6%. The phytated nanocellulose fibers are attached to the fiber surface through covalent bonds, interlaced and stacked with each other to form a porous network structure layer, and the coverage rate of the fiber surface is 95 to 100%.

[0035] The method for preparing a highly efficient flame-retardant fabric based on phytated nanocellulose fibers of the present invention comprises the following steps: first, synthesizing phytated nanocellulose fibers (PA-CNF) from phytic acid (PA) and nanocellulose fibers (CNF), and dispersing the synthesized nanocellulose fibers (PA-CNF) in deionized water. Then, the obtained dispersion is used to impregnate the fabric, and the wet weight of the fabric is controlled by rolling. Finally, baking and heating are performed to cause the phosphoric acid groups on the surface of the modified nanocellulose fibers to react chemically with the hydroxyl groups or amino groups on the surface of the fibers, thereby ensuring that the modified nanocellulose fibers are connected to the fibers through covalent bonds.

[0036] like Figure 1As shown, the method for preparing flame-retardant cotton fabric includes: firstly, covalently grafting phytic acid to nanocellulose fibers through an esterification reaction to obtain phytated nanocellulose fibers, and further esterifying the phosphoric acid groups on the phytated nanocellulose fibers with the hydroxyl groups on the surface of the cotton fibers to achieve chemical adsorption of a large amount of phytic acid components on the surface of the cotton fibers. The phytated nanocellulose fibers serve as flame retardants to impart flame retardant properties to the fabric.

[0037] The flame retardant cotton fabric preparation method comprises the following steps:

[0038] Step 1: Disperse the nanocellulose fibers in water, add phytic acid solution, and heat to react. After the reaction is completed, wash away the unreacted phytic acid small molecules to obtain phytated nanocellulose fibers;

[0039] Step 2: the phytated nanocellulose fibers are dispersed in deionized water, cotton fabric is immersed in deionized water, wet weight is controlled after taking out, heating reaction is carried out under hot pressing, ungrafted phytated nanofibers are washed off, and flame retardant cotton fabric is obtained after drying.

[0040] like Figure 2 As shown, the method for preparing flame-retardant polyester fabric includes: firstly, modifying polyester fabric by atomizing an organic amine solution to obtain aminated polyester fabric, and then grafting phytated nanocellulose fibers onto the fiber surface by an amidation reaction to impart flame-retardant properties.

[0041] The method for preparing flame retardant polyester fabric comprises the following steps:

[0042] Step 1, modifying polyester fabric using organic amine solution;

[0043] Step 2: Disperse phytated nanocellulose fibers in deionized water, immerse the polyester fabric therein, control the wet weight after taking it out, heat and react under hot pressure, elute the ungrafted phytated nanofibers with deionized water, and obtain the flame-retardant polyester fabric after drying.

[0044] Example 1

[0045] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose fibers.

[0046] The phytated nanocellulose fibers obtained above were dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at a temperature of 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0047] The LOI value of the flame-retardant cotton fabric was 36.2%, and the tensile strength was 31.1 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.3% and 34.2%. The moisture permeability of the flame-retardant cotton fabric was 4420 g / m 2 / d, the moisture absorption rate is 13.1%. Figure 3 As shown, the flame retardant cotton fabric prepared in Example 1 has a more obvious flame retardant effect than the original cotton fabric; Figure 4 As shown, the flame retardant cotton fabric prepared in Example 1 has no significant change in softness compared with the original fabric; Figure 5 As shown, the flame retardant cotton fabric prepared in Example 1 has significantly increased strength compared with the original cotton fabric; Figure 6 As shown, the coverage of the flame retardant layer is 99% according to SEM image statistics.

[0048] Example 2

[0049] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 6%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0050] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 2 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0051] The LOI value of the flame-retardant cotton fabric was 36.5%, and the tensile strength was 30.9 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.3% and 35.5%. The moisture permeability of the flame-retardant cotton fabric was 4440 g / m 2 / d, the moisture absorption rate is 13.6%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0052] Example 3

[0053] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 100°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0054] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0055] The LOI value of the flame-retardant cotton fabric was 36.6%, and the tensile strength was 30.7 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.4% and 35.7%. The moisture permeability of the flame-retardant cotton fabric was 4446 g / m 2 / d, the moisture absorption rate is 13.7%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0056] Example 4

[0057] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0058] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 6% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at a temperature of 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0059] The LOI value of the flame-retardant cotton fabric was 36.9%, and the tensile strength was 30.5 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.2% and 35.8%. The moisture permeability of the flame-retardant cotton fabric was 4458 g / m 2 / d, the moisture absorption rate is 13.8%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0060] Example 5

[0061] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0062] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 200%. The fabric was hot-pressed at a temperature of 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0063] The LOI value of the flame-retardant cotton fabric was 36.9%, and the tensile strength was 30.5 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.8% and 35.2%. The moisture permeability of the flame-retardant cotton fabric was 4473 g / m 2 / d, the moisture absorption rate is 13.9%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0064] Example 6

[0065] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0066] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. It was hot-pressed at a temperature of 200°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0067] The LOI value of the flame-retardant cotton fabric was 36.8%, and the tensile strength was 30.6 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.8% and 35.6%. The moisture permeability of the flame-retardant cotton fabric was 4462 g / m 2 / d, the moisture absorption rate is 13.8%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0068] Example 7

[0069] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0070] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 7 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0071] The LOI value of the flame-retardant cotton fabric was 36.8%, and the tensile strength was 30.5 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.4% and 35.4%. The moisture permeability of the flame-retardant cotton fabric was 4442 g / m 2 / d, the moisture absorption rate is 13.6%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0072] Example 8

[0073] Polyester fabric (2 g) was immersed in an ethanol solution of 2% aminopropyltriethoxysilane for 2 minutes with a bath ratio of 20 and a wet weight gain of 140%. After heating at 70°C for 5 minutes, the fabric was washed with deionized water and dried to obtain aminated polyester.

[0074] Phytated nanocellulose fibers (prepared in the same manner as in Example 1) were dispersed in deionized water to prepare a 4% dispersion. Amine polyester (2 g) was immersed in the dispersion for 3 minutes at a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was subjected to hot pressing at a temperature of 170°C for 5 minutes, washed with deionized water to remove the unsuccessfully covalently grafted phytated nanocellulose, and dried at 80°C to obtain a flame-retardant polyester cotton fabric.

[0075] The LOI value of the flame-retardant polyester fabric obtained is 36.5%, and the tensile strength is 43.5 MPa. After 120 washes or 1000 frictions, the LOI value is still 35.2% and 34.8%. The moisture permeability of the flame-retardant polyester fabric is 2400 g / m 2 / d, the moisture absorption rate is 4.2%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0076] Example 9

[0077] Polyester fabric (2 g) was immersed in an ethanol solution of 4% aminopropyltriethoxysilane for 2 minutes with a bath ratio of 20 and a wet weight gain of 140%. After heating at 70°C for 5 minutes, the fabric was washed with deionized water and dried to obtain aminated polyester.

[0078] Phytated nanocellulose (prepared in the same manner as in Example 1) was dispersed in deionized water to prepare a 4% dispersion. Aminated polyester (2 g) was immersed in it for 2 minutes, with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 200%, and the fabric was subjected to hot pressing at a temperature of 170°C for 2 minutes. The fabric was washed with deionized water to remove the unsuccessfully covalently grafted phytated nanocellulose, and dried at 80°C to obtain a flame-retardant polyester cotton fabric.

[0079] The LOI value of the flame-retardant polyester fabric obtained is 36.8%, and the tensile strength is 43.2 MPa. After 120 washes or 1000 frictions, the LOI value is still 35.5% and 35.2%. The moisture permeability of the flame-retardant polyester fabric is 2428 g / m 2 / d, the moisture absorption rate is 4.2%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0080] Example 10

[0081] Polyester fabric (2 g) was immersed in an ethanol solution of 2% aminopropyltriethoxysilane for 2 minutes with a bath ratio of 20 and a wet weight gain of 160%. After heating at 70°C for 5 minutes, the fabric was washed with deionized water and dried to obtain aminated polyester.

[0082] Phytated nanocellulose (prepared in the same manner as in Example 1) was dispersed in deionized water to prepare a 4% dispersion. Amine polyester (2 g) was immersed in it for 2 minutes, with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 200%. The fabric was subjected to hot pressing at 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant polyester cotton fabric.

[0083] The LOI value of the flame-retardant polyester fabric obtained is 36.8%, and the tensile strength is 43.3 MPa. After 120 washes or 1000 frictions, the LOI value is still 35.6% and 35.4%. The moisture permeability of the flame-retardant polyester fabric is 2428 g / m 2 / d, the moisture absorption rate is 4.3%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0084] Embodiment 11

[0085] Polyester fabric (2 g) was immersed in an ethanol solution of 2% aminopropyltriethoxysilane for 2 minutes with a bath ratio of 20 and a wet weight gain of 140%. After heating at 90°C for 5 minutes, the fabric was washed with deionized water and dried to obtain aminated polyester.

[0086] Phytated nanocellulose (prepared in the same manner as in Example 1) was dispersed in deionized water to prepare a 4% dispersion. Amine polyester (2 g) was immersed in it for 2 minutes, with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was subjected to hot pressing at a temperature of 170°C for 7 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant polyester cotton fabric.

[0087] The LOI value of the flame-retardant polyester fabric obtained was 36.9%, and the tensile strength was 43.2 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.1% and 34.9%. The moisture permeability of the flame-retardant polyester fabric was 2444 g / m 2 / d, the moisture absorption rate is 4.4%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0088] Comparative Example 1

[0089] 1 g of phytic acid was dissolved in deionized water to prepare a 0.05% solution. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 180%. The fabric was hot-pressed at 180°C for 5 minutes, washed with deionized water to remove the phytic acid that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0090] The LOI value of the flame retardant cotton fabric was 35.5%, the tensile strength was 8.2 MPa, and after 120 washes or 1000 frictions, the LOI values ​​were 33.2% and 32.8%. The moisture permeability of the flame retardant cotton fabric was 4000 g / m 2 / d, the moisture absorption rate is 11.2%.

[0091] Comparative Example 2

[0092] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 4% nanocellulose fiber dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. It was hot-pressed at a temperature of 170°C for 5 minutes, then washed with deionized water to remove the nanocellulose that was not successfully covalently grafted, and finally dried at 80°C to obtain a comparative cotton fabric.

[0093] The LOI value of the obtained cotton fabric is 18.9%, the tensile strength is 31.6 MPa, and after 120 washes or 1000 frictions, the LOI value is 18.9% and 18.9%. The moisture permeability of the obtained cotton fabric is 3530 g / m 2 / d, the moisture absorption rate is 8.5%. According to the SEM image statistics, the flame retardant layer coverage is 10%.

[0094] Comparative Example 3

[0095] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 3%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0096] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0097] The LOI value of the flame-retardant cotton fabric was 31.4%, and the tensile strength was 30.8 MPa. After 120 washes or 1000 frictions, the LOI value was still 29.2% and 29.8%. The moisture permeability of the flame-retardant cotton fabric was 4126 g / m 2 / d, the moisture absorption rate is 11.9%, and the flame retardant layer coverage is 97% according to SEM image statistics.

[0098] Comparative Example 4

[0099] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 7%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0100] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0101] The LOI value of the flame-retardant cotton fabric was 36.5%, and the tensile strength was 25.8 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.2% and 34.2%. The moisture permeability of the flame-retardant cotton fabric was 4421 g / m 2 / d, the moisture absorption rate is 13.8%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0102] Comparative Example 5

[0103] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 70°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0104] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0105] The LOI value of the flame-retardant cotton fabric was 30.7%, and the tensile strength was 30.9 MPa. After 120 washes or 1000 frictions, the LOI value was still 29.7% and 28.7%. The moisture permeability of the flame-retardant cotton fabric was 3888 g / m 2 / d, the moisture absorption rate is 9.2%, and the flame retardant layer coverage is 94% according to SEM image statistics.

[0106] Comparative Example 6

[0107] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0108] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 3% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at a temperature of 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0109] The LOI value of the flame-retardant cotton fabric was 30.3%, and the tensile strength was 30.9 MPa. After 120 washes or 1000 frictions, the LOI value was still 28.6% and 29.1%. The moisture permeability of the flame-retardant cotton fabric was 3762 g / m 2 / d, the moisture absorption rate is 9.1%, and the flame retardant layer coverage is 93% according to SEM image statistics.

[0110] Comparative Example 7

[0111] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0112] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 160%. The fabric was hot-pressed at a temperature of 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0113] The LOI value of the flame retardant cotton fabric was 30.7%, and the tensile strength was 30.7 MPa. After 120 washes or 1000 frictions, the LOI value was still 29.6% and 29.1%. The moisture permeability of the flame retardant cotton fabric was 3918 g / m 2 / d, the moisture absorption rate is 9.4%, and the flame retardant layer coverage is 92% according to SEM image statistics.

[0114] Comparative Example 8

[0115] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0116] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, the bath ratio was 20, and the wet weight of the fabric was controlled to be 170% after being taken out. The fabric was hot-pressed at a temperature of 160°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0117] The LOI value of the flame-retardant cotton fabric was 29.9%, and the tensile strength was 30.9 MPa. After 120 washes or 1000 frictions, the LOI value was still 28.4% and 27.2%. The moisture permeability of the flame-retardant cotton fabric was 3721 g / m 2 / d, the moisture absorption rate is 9.1%, and the coverage of the flame retardant layer is 90% according to SEM image statistics.

[0118] Comparative Example 9

[0119] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0120] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 1 minute, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0121] The LOI value of the flame-retardant cotton fabric was 33.6%, and the tensile strength was 30.4 MPa. After 120 washes or 1000 frictions, the LOI value was still 30.8% and 30.2%. The moisture permeability of the flame-retardant cotton fabric was 4033 g / m 2 / d, the moisture absorption rate is 11.5%, and the flame retardant layer coverage is 96% according to SEM image statistics.

[0122] Comparative Example 10

[0123] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0124] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 7% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, with a bath ratio of 20. After taking it out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at a temperature of 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0125] The LOI value of the flame-retardant cotton fabric was 36.7%, and the tensile strength was 26.9 MPa. After 120 washes or 1000 frictions, the LOI value was still 35.8% and 35.2%. The moisture permeability of the flame-retardant cotton fabric was 4423 g / m 2 / d, the moisture absorption rate is 13.6%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0126] Comparative Example 11

[0127] 5 g of nanocellulose fibers were stirred and dispersed in water to prepare a 2% nanocellulose fiber dispersion, and phytic acid was added to control its concentration to 4%. The mixture was heated at 80°C for 4 hours, centrifuged at 5000 rpm for 10 minutes, and the supernatant was removed. The obtained fibers were washed with deionized water to remove unreacted phytic acid small molecules, thereby obtaining phytated nanocellulose.

[0128] The phytated nanocellulose obtained above was dispersed in deionized water to prepare a 4% dispersion. 2 g of cotton fabric was immersed in it for 2 minutes, the bath ratio was 20, and the wet weight of the fabric was controlled to be 210% after being taken out. The fabric was hot-pressed at a temperature of 170°C for 5 minutes, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant cotton fabric.

[0129] The LOI value of the flame-retardant cotton fabric was 36.4%, and the tensile strength was 25.1 MPa. After 120 washes or 1000 frictions, the LOI value was still 33.4% and 32.6%. The moisture permeability of the flame-retardant cotton fabric was 4444 g / m 2 / d, the moisture absorption rate is 13.7%, and the flame retardant layer coverage is 99% according to SEM image statistics.

[0130] Comparative Example 12

[0131] Polyester fabric (2 g) was immersed in an ethanol solution of 1% aminopropyltriethoxysilane for 2 minutes with a bath ratio of 20 and a wet weight gain of 140%. After heating at 70°C for 5 minutes, the fabric was washed with deionized water and dried to obtain aminated polyester.

[0132] Phytated nanocellulose (prepared in the same manner as in Example 1) was dispersed in deionized water to prepare a dispersion with a mass fraction of 4%. Amine polyester (2 g) was immersed in it for 2 minutes with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, then washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and finally dried at 80°C to obtain a flame-retardant polyester fabric.

[0133] The LOI value of the flame retardant polyester fabric was 25.1%, the tensile strength was 43.6 MPa, and after 120 washes or 1000 frictions, the LOI values ​​were 23.9% and 23.8%. The moisture permeability of the flame retardant polyester fabric was 1988 g / m 2 / d, the moisture absorption rate is 2.1%, and the flame retardant layer coverage is 92% according to SEM image statistics.

[0134] Comparative Example 13

[0135] Polyester fabric (2 g) was immersed in an ethanol solution of 2% aminopropyltriethoxysilane for 2 minutes with a bath ratio of 20 and a wet weight gain of 130%. After heating at 70°C for 5 minutes, the fabric was washed with deionized water and dried to obtain aminated polyester.

[0136] Phytated nanocellulose (prepared in the same manner as in Example 1) was dispersed in deionized water to prepare a dispersion with a mass fraction of 4%. Amine polyester (2 g) was immersed in it for 2 minutes with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, then washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and finally dried at 80°C to obtain a flame-retardant polyester fabric.

[0137] The LOI value of the flame retardant polyester fabric was 32.8%, the tensile strength was 43.7 MPa, and after 120 washes or 1000 frictions, the LOI values ​​were 30.2% and 30.9%. The moisture permeability of the flame retardant polyester fabric was 2246 g / m 2 / d, the moisture absorption rate is 2.6%, and the flame retardant layer coverage is 95% according to SEM image statistics.

[0138] Comparative Example 14

[0139] Polyester fabric (2 g) was immersed in an ethanol solution of 2% aminopropyltriethoxysilane for 2 minutes with a bath ratio of 20 and a wet weight gain of 140%. After heating at 60°C for 5 minutes, the fabric was washed with deionized water and dried to obtain aminated polyester.

[0140] Phytated nanocellulose (prepared in the same manner as in Example 1) was dispersed in deionized water to prepare a dispersion with a mass fraction of 4%. Amine polyester (2 g) was immersed in it for 2 minutes with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, then washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and finally dried at 80°C to obtain a flame-retardant polyester fabric.

[0141] The LOI value of the flame retardant polyester fabric was 28.2%, the tensile strength was 43.6 MPa, and after 120 washes or 1000 frictions, the LOI values ​​were 26.3% and 26.1%. The moisture permeability of the flame retardant polyester fabric was 2012 g / m 2 / d, the moisture absorption rate is 2.4%, and the flame retardant layer coverage is 93% according to SEM image statistics.

[0142] Comparative Example 15

[0143] Polyester fabric (2 g) was immersed in an ethanol solution of 2% aminopropyltriethoxysilane for 2 minutes with a bath ratio of 20 and a wet weight gain of 140%. After heating at 70°C for 4 minutes, the fabric was washed with deionized water and dried to obtain aminated polyester.

[0144] Phytated nanocellulose (prepared in the same manner as in Example 1) was dispersed in deionized water to prepare a dispersion with a mass fraction of 4%. Amine polyester (2 g) was immersed in it for 2 minutes with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, then washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and finally dried at 80°C to obtain a flame-retardant polyester fabric.

[0145] The LOI value of the flame retardant polyester fabric was 32.8%, the tensile strength was 43.6 MPa, and after 120 washes or 1000 frictions, the LOI values ​​were 31.4% and 31.2%. The moisture permeability of the flame retardant polyester fabric was 2199 g / m 2 / d, the moisture absorption rate is 2.5%, and the flame retardant layer coverage is 94% according to SEM image statistics.

[0146] Comparative Example 16

[0147] 1 g of phytic acid was dissolved in deionized water to prepare a 0.05% solution. Polyester fabric (2 g) was immersed in it for 2 minutes with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was hot-pressed at 170°C for 5 minutes, washed with deionized water to remove the phytic acid that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant polyester fabric.

[0148] The LOI value of the flame retardant polyester fabric was 36.4%, the tensile strength was 15.2 MPa, and after 120 washes or 1000 frictions, the LOI values ​​were 35.3% and 34.2%. The moisture permeability of the flame retardant polyester fabric was 1952 g / m 2 / d, the moisture absorption rate is 2.3%.

[0149] Comparative Example 17

[0150] Phytated nanocellulose (prepared in the same manner as in Example 1) was dispersed in deionized water to prepare a 4% dispersion. Polyester fabric (2 g) was immersed in it for 2 minutes with a bath ratio of 20. After being taken out, the wet weight of the fabric was controlled to be 170%. The fabric was subjected to hot pressing for 5 minutes at a temperature of 170°C, washed with deionized water to remove the phytated nanocellulose that was not successfully covalently grafted, and dried at 80°C to obtain a flame-retardant polyester fabric.

[0151] The LOI value of the flame-retardant polyester fabric obtained is 23.1%, and the tensile strength is 44.2 MPa. After 120 washes or 1000 frictions, the LOI value is still 22.8% and 22.6%. The moisture permeability of the flame-retardant polyester fabric is 1600 g / m 2 / d, the moisture absorption rate is 0.8%, and the coverage of the flame retardant layer is 10% according to SEM image statistics.

[0152] The preparation conditions and product performance characterization results of each embodiment and comparative example are shown in Table 1, Table 2 and Table 3 below.

[0153] Table 1 Preparation conditions of flame retardant cotton fabrics.

[0154]

[0155] Table 2 Preparation conditions of flame retardant polyester.

[0156]

[0157] Table 3 Product performance characterization results.

[0158]

[0159]

[0160] The present invention adopts the esterification reaction between the phosphoric acid group of phytic acid and the hydroxyl group of nanocellulose fiber, and the phytic acid grafting gives the nanocellulose fiber a flame retardant function. The phosphoric acid group on the phytated nanocellulose fiber further undergoes an esterification reaction with the hydroxyl group on the surface of the cotton fiber to achieve covalent grafting, thereby achieving flame retardancy of the cotton fabric. The phosphoric acid group on the phytated nanocellulose fiber undergoes an amidation reaction with the polyester fiber treated with an organic amine to achieve chemical grafting, giving the polyester fabric flame retardant properties. Since the phytated nanocellulose fiber has a larger volume than the phytic acid molecule, it is not easy to penetrate into the fiber core, thereby effectively inhibiting the degradation of the polymer in the fiber to ensure the mechanical strength of the fabric.

[0161] The above description and the figures are only preferred embodiments of the present invention. It should be noted that, for those skilled in the art, several modifications and improvements can be made without departing from the principle of the present invention, which should also be considered to belong to the protection scope of the present invention.

Claims

1. A highly effective flame retardant fabric based on phytated nanocellulose fibers, wherein the phosphorus content of the phytated nanocellulose fibers is 4-6%, characterized in that: The phytated nanocellulose fibers are attached to the surface of the fabric fibers through covalent bonds to form a porous network structure layer, and the porous network structure layer constitutes a flame retardant layer.

2. The high-efficiency flame-retardant fabric based on phytated nanocellulose fibers according to claim 1, characterized in that: The fabric is cotton fabric.

3. A method for preparing a highly effective flame-retardant fabric based on phytated nanocellulose fibers according to claim 2, characterized in that The steps include: Step 1: dispersing the nanocellulose fibers in water, adding a phytic acid solution, heating for reaction, and washing away unreacted phytic acid small molecules after the reaction to obtain phytated nanocellulose fibers; Step 2: dispersing the phytated nanocellulose fibers in deionized water to prepare a dispersion, immersing cotton fabric in the dispersion, controlling the wet weight after taking it out, heating and reacting under hot pressure, washing away the ungrafted phytated nanocellulose fibers, and drying to obtain a flame-retardant cotton fabric.

4. The preparation method according to claim 3, characterized in that: In step 1, the mass fraction of the solution after the nanocellulose fibers are dispersed is 2-3%, the mass fraction of the phytic acid solution is 4-6%, the reaction temperature is 80-100° C., and the reaction time is 4-5 hours.

5. The preparation method according to claim 3, characterized in that: The mass fraction of the dispersion in step 2 is 4-6%, the immersion treatment time is 2-3 minutes, the wet weight is controlled to be 170-200%, the reaction temperature is 170-200° C., and the time is 2-7 minutes.

6. The high-efficiency flame-retardant fabric based on phytated nanocellulose fibers according to claim 1, characterized in that: The fabric is polyester fabric.

7. A method for preparing a highly effective flame retardant fabric based on phytated nanocellulose fibers according to claim 6, characterized in that The steps include: Step 1: using an organic amine solution to modify polyester fabric to obtain aminated polyester; Step 2: dispersing the nanocellulose fibers in water, adding phytic acid solution, heating for reaction, and washing away unreacted phytic acid small molecules after the reaction to obtain phytated nanocellulose fibers; Step 3: dispersing the phytated nanocellulose fibers in deionized water to prepare a dispersion, immersing the aminated polyester in the dispersion, controlling the wet weight after taking it out, heating and reacting under hot pressure, washing away the ungrafted phytated nanocellulose fibers, and drying to obtain a flame-retardant polyester fabric.

8. The preparation method according to claim 7, characterized in that: The organic amine solution in step 1 is an aminopropyltriethoxysilane solution with a mass fraction of 2-4%. The polyester fabric is immersed in the solution for 2-3 minutes, the wet weight is controlled to be 140-160%, the temperature is raised to 70-90°C, and the reaction is carried out for 5-10 minutes.

9. The preparation method according to claim 7, characterized in that: In step 2, the mass fraction of the solution after the nanocellulose fibers are dispersed is 2-3%, the mass fraction of the phytic acid solution is 4-6%, the reaction temperature is 80-100° C., and the reaction time is 4-5 hours.

10. The preparation method according to claim 7, characterized in that: The mass fraction of the dispersion in step 3 is 4-6%, the immersion treatment time is 2-3 minutes, the wet weight is controlled to be 170-200%, the reaction temperature is 170-200°C, and the time is 2-7 minutes.

Citation Information

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