Preparation method of durable flame-retardant, antibacterial and multifunctional modified polyester / cotton blended fabric
By synthesizing a multifunctional modifier containing aromatic groups and phosphate in a polyester/cotton blended fabric, and fixing the flame retardant by covalent grafting reaction, the problems of flame retardant effect and durability of polyester/cotton blended fabrics are solved, and high-efficiency and durable flame retardant and antibacterial properties are achieved.
Patent Information
- Application Number
- CN202311131489.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-04
- Publication Date
- 2025-08-26
- Estimated Expiration
- 2043-09-04
AI Technical Summary
The prior art is difficult to covalently crosslink the DOPO-based flame retardant with cotton fibers and polyester fibers, resulting in insufficient flame retardant effect and durability of polyester/cotton blended fabrics.
The reaction of aniline and terephthalaldehyde was used to form the Schiff base structure, and the P-H bonds of phosphoric acid and DOPO were reacted with the Schiff base structure to undergo Pudovik addition reaction, to synthesize a multifunctional modifier containing aromatic groups and phosphate, and the polyester/cotton blended fabric was treated by impregnation-baking method, and the flame retardant was fixed by catalyzed covalent graft reaction.
The durable flame retardant and antibacterial properties of polyester/cotton blended fabrics are achieved, the flame retardant efficiency and antibacterial effect are improved, and the good performance remains after multiple washes.
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Figure CN117385637B_ABST
Abstract
Description
Technical field
[0001] The invention belongs to the technical field of textiles and relates to a method for preparing a durable flame-retardant, antibacterial and multifunctional modified polyester / cotton blended fabric. [Background Technology]
[0002] Polyester / cotton blended fabrics offer exceptional performance, with the complementary properties of cotton and polyester fibers providing a combination of stiffness, wear resistance, moisture permeability, and comfort. They are widely used in clothing, bedding, and interior decoration. However, polyester / cotton blends exhibit a "wicking effect" during combustion, resulting in more intense combustion than single polyester or cotton components. While extensive research has been conducted domestically and internationally on flame-retardant finishing of polyester / cotton blends, the flame-retardant efficiency and durability of these finished fabrics remain to be further improved.
[0003] 9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) flame retardant is a halogen-free, environmentally friendly, and highly effective phosphorus-containing flame retardant. It is primarily used in synthetic fibers such as flame-retardant polyester through blending and addition. While post-finishing methods offer simplicity, convenience, and flexibility, producing durable, flame-retardant polyester / cotton blended fabrics using DOPO through this process presents significant challenges.
[0004] Reference (DOPO-hydroxymethyl derivative flame retardant finishing of polyester fabric [J]. Printing and Dyeing, 2016, 42(19): 6-10, 20) uses DOPO and its hydroxymethyl derivatives to flame retardant finish polyester fabric by high temperature and high pressure method, giving polyester fabric good flame retardant properties; however, the DOPO and its hydroxymethyl derivatives mainly improve the flame retardant properties of polyester through the gas phase flame retardant mechanism, but have poor flame retardant effect on polyester / cotton blended fabrics, and cannot form covalent bonds with cotton fibers, and cannot achieve good flame retardant effect and water washability. Chinese invention patent CN103881134A discloses a DOPO-derived phosphorus-nitrogen flame retardant and its preparation method and application. The DOPO-derived phosphorus-nitrogen flame retardant is synthesized using DOPO and N-hydroxymethyl acrylamide. The flame retardant properties of the DOPO-derived phosphorus-nitrogen flame retardant are good for epoxy resin. However, the flame retardant cotton fabric only reaches UL94 V-1 level, and the flame retardant properties are poor.
[0005] There are great challenges in developing a DOPO-based flame retardant that can both covalently cross-link with cotton fibers and interact with polyester fibers. [Summary of the invention]
[0006] In order to solve the above technical problems and overcome the shortcomings of the existing technical books, the present invention provides a method for preparing a durable flame retardant and antibacterial multifunctional modified polyester / cotton blended fabric, wherein the prepared fabric has durable flame retardant and antibacterial functions.
[0007] In order to achieve the above purpose, the following technical solutions are adopted:
[0008] A method for preparing a durable flame-retardant, antibacterial, multifunctional modified polyester / cotton blended fabric comprises the following steps:
[0009] S1. Aniline and terephthalaldehyde are dissolved in ethanol and reacted at 80-90°C for 3-4 hours. P-phenylenediamine, phosphorous acid and DOPO are added in sequence and the reaction is continued for 5-7 hours. After the reaction, the mixture is subjected to reduced pressure distillation and washing to obtain a multifunctional modifier containing an aromatic group, a phosphate group and a Schiff base structure.
[0010] S2. Add the multifunctional modifier, ammonia water, dicyandiamide, dispersant NNO and penetrant JFC into the aqueous solution and disperse them for 2 to 3 hours using a high-speed shear emulsifier to prepare a flame retardant dispersion.
[0011] S3. Treating the polyester / cotton blended fabric by an impregnation-baking method to obtain a durable, flame-retardant, antibacterial and multifunctional polyester / cotton blended fabric.
[0012] Furthermore, in step S1, the molar ratio of aniline to terephthalaldehyde is 1:1.2-1.3, the mass ratio of terephthalaldehyde to ethanol is 1:30-50, the molar ratio of p-phenylenediamine to terephthalaldehyde is 1-1.2:2, the molar ratio of phosphorous acid to terephthalaldehyde is 1-1.2:1, and the molar ratio of DOPO to terephthalaldehyde is 1-1.2:1.
[0013] Furthermore, in step S2, the rotation speed of the high-speed shear emulsifier is 3000-5000 rpm.
[0014] Furthermore, in step S2, the concentration of the multifunctional modifier is 200-300 g / L, the amount of the dispersant NNO is 4-6% of the mass of the flame retardant dispersion, the amount of the penetrant JFC is 3-5 g / L, and the amount of dicyandiamide is 40-60 g / L;
[0015] The pH value of the flame retardant dispersion is 6-8.
[0016] Furthermore, step S3 specifically includes the following steps:
[0017] S31, immersing the polyester / cotton blended fabric in the flame retardant dispersion for padding, wherein the liquid carrying rate of the polyester / cotton blended fabric after padding is 90-110%;
[0018] S32. Pre-drying and baking the impregnated polyester / cotton blended fabric in sequence, wherein the pre-drying temperature is 70-90° C. for 1-2 min, and the baking temperature is 180-200° C. for 2-4 min.
[0019] Furthermore, in step S3, the polyester / cotton blended fabric is a polyester / cotton blended fabric with a ratio of 40 / 60, 45 / 55, 65 / 35 or 80 / 20.
[0020] Compared with the prior art, the present invention has the following advantages:
[0021] (1) The present invention synthesizes a multifunctional modifier containing an aromatic group, a phosphate group, and a Schiff base structure by allowing the amino groups of p-phenylenediamine and aniline to react with the aldehyde group of terephthalaldehyde through a Schiff base reaction, and the pH bond of phosphorous acid and DOPO to react with the Schiff base C=N structure through a Pudovik addition reaction. First, the multifunctional modifier contains an aromatic structure and has a strong affinity with polyester fibers. During the high-temperature baking process, the instantaneous gaps in the polyester fibers open, allowing the multifunctional modifier molecules to diffuse into the interior of the polyester fibers and bind to the polyester fibers through the principle of like dissolves like. In addition, the ammonium phosphate structure in the multifunctional modifier molecules undergoes a covalent grafting reaction with the active hydroxyl groups of the cotton fibers under the catalysis of dicyandiamide, so that the flame retardant can be firmly fixed to the polyester fibers and cotton fibers, thereby providing durable flame retardant and antibacterial functions.
[0022] (2) The preparation method of the present invention provides a flame retardant molecule comprising phosphorus-containing flame retardant groups, Schiff base C=N structures, and aromatic benzene rings, which can produce a synergistic flame retardant effect, effectively promoting the charring of polyester / cotton blended fabrics and exhibiting high flame retardant efficiency. Furthermore, the Schiff base structure exhibits high biological activity, imparting excellent antibacterial properties to the modified polyester / cotton blended fabric.
Brief Description of the Drawings
[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.
[0024] Figure 1 This is an infrared spectrum of the flame retardant containing aromatic groups and phosphate groups prepared in Example 1 of the present invention;
[0025] Figure 2 1 is the heat release rate curve of the unmodified and durable flame retardant modified polyester / cotton blended fabrics prepared in Example 1 of the present invention after microcalorimetry testing. [Specific implementation method]
[0026] To further help understand the technical solution of the present invention, the technical solution of the present invention is described in more detail below by providing several specific implementation examples. All of the described embodiments are only partial embodiments of the present invention, not all of them. The following specific embodiments can be combined with each other, and the same or similar concepts or processes therein may not be repeated in some embodiments.
[0027] Example 1
[0028] The experimental chemicals used in this embodiment are: aniline, terephthalaldehyde, terephthalaldehyde, ethanol, p-phenylenediamine, phosphorous acid, flame retardant DOPO, ammonia, dicyandiamide, dispersant NNO and penetrant JFC. The base fabric used in this embodiment is a 40 / 60 polyester / cotton blended fabric.
[0029] (1) Aniline and terephthalaldehyde are dissolved in ethanol, heated to 80°C and refluxed for 3 hours, then p-phenylenediamine, phosphorous acid and flame retardant DOPO are added in sequence, and the reaction is continued at 80°C for 5 hours. After vacuum distillation and ethanol washing, a multifunctional modifier containing aromatic groups, phosphate groups and Schiff base structures is obtained. In this step (1), the molar ratio of aniline to terephthalaldehyde is 1:1.2, the mass ratio of terephthalaldehyde to ethanol is 1:30, the molar ratio of p-phenylenediamine to terephthalaldehyde is 1:2, the molar ratio of phosphorous acid to terephthalaldehyde is 1:1, and the molar ratio of DOPO to terephthalaldehyde is 1:1. p-phenylenediamine, aniline and terephthalaldehyde undergo a Schiff base reaction, and the PH bond of phosphorous acid and DOPO can undergo a Pudovik addition reaction with the Schiff base structure.
[0030] The yield of the multifunctional modifier prepared in step (1) is 78%. The structure of the multifunctional modifier is as follows (1):
[0031]
[0032] (2) Add the multifunctional modifier, ammonia water, dicyandiamide, dispersant NNO and penetrant JFC to the aqueous solution, use a high-speed shear emulsifier to disperse for 3 hours, and prepare a flame retardant dispersion for 3 hours, wherein the speed of the high-speed shear emulsifier is 5000rpm. In this step (2), the mass of the flame retardant dispersion can be determined first according to actual needs, and then the amount of the multifunctional modifier, dispersant NNO, penetrant JFC and dicyandiamide is calculated based on the predetermined mass of the flame retardant dispersion, and then the pH value of the flame retardant dispersion is adjusted to 6 by ammonia water. In this step (2), the amount of dispersant NNO is 4% of the mass of the flame retardant dispersion, the amount of penetrant JFC is 3g / L, the concentration of the multifunctional modifier is 200g / L, and the amount of dicyandiamide is 40g / L. By using ammonia water to adjust the pH value of the dispersion to 6, the multifunctional modifier generates an ammonium phosphate structure. Dicyandiamide can catalyze the covalent grafting reaction between the multifunctional modifier ammonium phosphate and the hydroxyl groups of cotton fibers.
[0033] (3) A 40 / 60 polyester / cotton blended fabric was immersed in a flame retardant dispersion for impregnation and pressing, and the impregnated polyester / cotton blended fabric was pre-baked and baked in sequence, wherein the pre-baking temperature was 70°C for 2 minutes, and the baking temperature was 180°C for 4 minutes, to obtain a high-efficiency, durable, flame-retardant, antibacterial and multifunctional polyester / cotton blended fabric.
[0034] Example 2
[0035] The experimental chemicals used in this Example 2 are the same as those in Example 1. The base fabric used in this Example is a 45 / 55 polyester / cotton blended fabric.
[0036] (1) Aniline and terephthalaldehyde are dissolved in ethanol, heated to 90°C and refluxed for 3 hours, then p-phenylenediamine, phosphorous acid and flame retardant DOPO are added in sequence, and the reaction is continued at 90°C for 5 hours. After vacuum distillation and ethanol washing, a multifunctional modifier containing aromatic groups, phosphate groups and Schiff base structures is obtained. In step (1), the molar ratio of aniline to terephthalaldehyde is 1:1.3, the mass ratio of terephthalaldehyde to ethanol is 1:50, the molar ratio of p-phenylenediamine to terephthalaldehyde is 1.2:2, the molar ratio of phosphorous acid to terephthalaldehyde is 1.2:1, and the molar ratio of DOPO to terephthalaldehyde is 1.2:1. In this step, p-phenylenediamine, aniline and terephthalaldehyde undergo Schiff base reaction, and the PH bond of phosphorous acid and DOPO can undergo Pudovik addition reaction with the Schiff base structure.
[0037] The yield of the multifunctional modifier prepared in step (1) is 75%. The structure of the multifunctional modifier is as follows (1):
[0038]
[0039] (2) Add the multifunctional modifier, ammonia water, dicyandiamide, dispersant NNO and penetrant JFC to the aqueous solution and disperse them for 2 hours using a high-speed shear emulsifier to prepare a flame retardant dispersion, wherein the speed of the high-speed shear emulsifier is 5000 rpm. In this step (2), the mass of the flame retardant dispersion can be determined first according to actual needs, and then the amount of the multifunctional modifier, dispersant NNO, penetrant JFC and dicyandiamide can be calculated based on the predetermined mass of the flame retardant dispersion, and then the pH value of the flame retardant dispersion is adjusted to 8 using ammonia water. In this step (2), the amount of dispersant NNO is 6% of the mass of the flame retardant dispersion, the amount of penetrant JFC is 5g / L, the concentration of the multifunctional modifier is 230g / L, and the amount of dicyandiamide is 60g / L. By adjusting the pH value of the dispersion to 8 using ammonia water, the multifunctional modifier generates an ammonium phosphate structure. Dicyandiamide can catalyze the covalent grafting reaction between the ammonium phosphate group of the multifunctional modifier and the hydroxyl group of the cotton fiber.
[0040] (3) A 45 / 55 polyester / cotton blended fabric was immersed in a flame retardant dispersion for impregnation and pressing, and the impregnated polyester / cotton blended fabric was pre-baked and baked in sequence, wherein the pre-baking temperature was 80°C for 1.5 min, and the baking temperature was 190°C for 3 min, to obtain a high-efficiency, durable, flame-retardant, antibacterial and multifunctional polyester / cotton blended fabric.
[0041] Example 3
[0042] The experimental chemicals used in this Example 3 are the same as those in Example 1. The base fabric used in this Example is a 65 / 35 polyester / cotton blended fabric.
[0043] (1) Aniline and terephthalaldehyde are dissolved in ethanol, heated to 85°C and refluxed for 3.5 hours, then p-phenylenediamine, phosphorous acid and flame retardant DOPO are added in sequence, and the reaction is continued at 85°C for 6 hours. After vacuum distillation and ethanol washing, a multifunctional modifier containing aromatic groups, phosphate groups and Schiff base structures is obtained. In step (1), the molar ratio of aniline to terephthalaldehyde is 1:1.2, the mass ratio of terephthalaldehyde to ethanol is 1:40, the molar ratio of p-phenylenediamine to terephthalaldehyde is 1.1:2, the molar ratio of phosphorous acid to terephthalaldehyde is 1:1, and the molar ratio of DOPO to terephthalaldehyde is 1:1. In this step, p-phenylenediamine, aniline and terephthalaldehyde undergo Schiff base reaction, and the PH bond of phosphorous acid and DOPO can undergo Pudovik addition reaction with the Schiff base structure.
[0044] The yield of the multifunctional modifier prepared in step (1) is 73%. The structure of the multifunctional modifier is as follows (1):
[0045]
[0046] (2) The multifunctional modifier, ammonia water, dicyandiamide, dispersant NNO and penetrant JFC are dispersed in an aqueous solution to prepare a flame retardant dispersion, and the dispersion is carried out for 2.5 hours using a high-speed shear emulsifier at a speed of 4000 rpm. In this step (2), the mass of the flame retardant dispersion can be determined first according to actual needs, and then the amount of the multifunctional modifier, dispersant NNO, penetrant JFC and dicyandiamide is calculated based on the predetermined mass of the flame retardant dispersion, and then the pH value of the flame retardant dispersion is adjusted to 6 using ammonia water. In this step (2), the amount of dispersant NNO is 5% of the mass of the flame retardant dispersion, the amount of penetrant JFC is 4 g / L, the concentration of the multifunctional modifier is 250 g / L, and the amount of dicyandiamide is 50 g / L. By adjusting the pH value of the dispersion to 7 using ammonia water, the multifunctional modifier generates an ammonium phosphate structure. Dicyandiamide can catalyze the covalent grafting reaction between the ammonium phosphate group of the multifunctional modifier and the hydroxyl group of the cotton fiber.
[0047] (3) A 65 / 35 polyester / cotton blended fabric was immersed in a flame retardant dispersion for impregnation and pressing, and the impregnated polyester / cotton blended fabric was pre-baked and baked in sequence, wherein the pre-baking temperature was 90°C for 1 min, and the baking temperature was 200°C for 2 min, to obtain a high-efficiency, durable, flame-retardant, antibacterial and multifunctional polyester / cotton blended fabric.
[0048] Example 4
[0049] The experimental chemicals used in this Example 4 are the same as those in Example 1. The base fabric used in this Example is an 80 / 20 polyester / cotton blended fabric.
[0050] (1) Aniline and terephthalaldehyde are dissolved in ethanol, heated to 80°C and refluxed for 4 hours, then p-phenylenediamine, phosphorous acid and flame retardant DOPO are added in sequence, and the reaction is continued at 80°C for 7 hours. After vacuum distillation and ethanol washing, a multifunctional modifier containing aromatic groups, phosphate groups and Schiff base structures is obtained. In step (1), the molar ratio of aniline to terephthalaldehyde is 1:1.2, the mass ratio of terephthalaldehyde to ethanol is 1:50, the molar ratio of p-phenylenediamine to terephthalaldehyde is 1.2:2, the molar ratio of phosphorous acid to terephthalaldehyde is 1.2:1, and the molar ratio of DOPO to terephthalaldehyde is 1.:1. In this step, p-phenylenediamine, aniline and terephthalaldehyde undergo Schiff base reaction, and the PH bond of phosphorous acid and DOPO can undergo Pudovik addition reaction with the Schiff base structure.
[0051] The yield of the multifunctional modifier prepared in step (1) is 73%. The structure of the multifunctional modifier is as follows (1):
[0052]
[0053] (2) The multifunctional modifier, ammonia water, dicyandiamide, dispersant NNO and penetrant JFC are dispersed in an aqueous solution to prepare a flame retardant dispersion, and the dispersion is carried out for 2 hours using a high-speed shear emulsifier at a speed of 3000 rpm. In this step (2), the mass of the flame retardant dispersion can be determined first according to actual needs, and then the amount of the multifunctional modifier, dispersant NNO, penetrant JFC and dicyandiamide is calculated based on the predetermined mass of the flame retardant dispersion, and then the pH value of the flame retardant dispersion is adjusted to 6 using ammonia water. In this step (2), the amount of dispersant NNO is 4% of the mass of the flame retardant dispersion, the amount of penetrant JFC is 3 g / L, the concentration of the multifunctional modifier is 300 g / L, and the amount of dicyandiamide is 40 g / L. By adjusting the pH value of the dispersion to 6 using ammonia water, the multifunctional modifier generates an ammonium phosphate structure. Dicyandiamide can catalyze the covalent grafting reaction between the ammonium phosphate group of the multifunctional modifier and the hydroxyl group of the cotton fiber.
[0054] (3) An 80 / 20 polyester / cotton blended fabric was immersed in a flame retardant dispersion for impregnation and pressing, and the impregnated polyester / cotton blended fabric was pre-baked and baked in sequence, wherein the pre-baking temperature was 85°C and the time was 1.5 min, and the baking temperature was 195°C and the time was 3 min, thereby obtaining a high-efficiency, durable, flame-retardant, antibacterial and multifunctional polyester / cotton blended fabric.
[0055] Comparative Example
[0056] The original sample selected for the comparative example is a 40 / 60 polyester / cotton blended fabric that has not been modified by the preparation method of the present invention.
[0057] The following describes the test indicators of the durable flame retardant and antibacterial polyester / cotton blended fabric prepared in the embodiment of the present invention. The durable flame retardant and antibacterial polyester / cotton blended fabric prepared in the present invention is evaluated using the following indicators.
[0058] Limiting oxygen index: GB / T 5454-1997 "Textile combustion performance test oxygen index method" is used to test the limiting oxygen index of modified polyester / cotton blended fabrics.
[0059] Damage length: GB / T 5455-2014 “Fire performance of textiles - Determination of damage length in vertical direction - Smoldering and afterflaming time” was used to test the damage length of modified polyester / cotton blended fabrics.
[0060] Antibacterial rate test: According to GB / T 20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method", the antibacterial rate of modified polyester / cotton blended fabric against Escherichia coli and Staphylococcus aureus was tested.
[0061] The above test standards were used for testing. The indicators of the durable flame retardant and antibacterial polyester / cotton blended fabrics prepared in various embodiments of the present invention are shown in Table 1.
[0062] Table 1
[0063]
[0064] As can be seen from Table 1, the durable flame-retardant polyester / cotton blended fabric of the present invention has a limiting oxygen index higher than 29.1%, a damaged length lower than 12.2 cm (the damaged length of the polyester / cotton blended fabric before flame retardant modification is 30 cm, and the LOI is approximately 17.1%), and the damaged length is no more than 14.7 cm after 30 washes. The antibacterial rates against Escherichia coli and Staphylococcus aureus are 91.1-99.9%.
[0065] See also Figure 1 , which is the infrared spectrum of the flame retardant containing aromatic groups and phosphate groups prepared in Example 1. Figure 1 As shown, 3423 and 3135cm -1 The absorption peaks at 2917 and 2849 cm are caused by the stretching vibration of NH and aromatic CH. -1 The absorption peaks at 1699 and 1154 cm are caused by the stretching vibration of methyl CH. -1 The absorption peak at 1402cm is caused by the stretching vibration of the Schiff base C=N and CN structure. -1 The absorption peaks at 1296, 1220, 1109 and 943 cm are caused by the bending vibration of aromatic CH. -1 The absorption peak at is caused by the stretching vibration of OPO, P=O, PO and POC groups in the structure of DOPO and phosphoric acid. The above results indicate that the flame retardant containing aromatic groups and phosphate groups was successfully synthesized.
[0066] See also Figure 2 , which is the heat release rate curve of the unmodified and durable flame retardant modified polyester / cotton blended fabrics prepared in Example 1 of the present invention after microcalorimetry testing. Figure 2 As shown in the figure, the unmodified polyester / cotton blended fabric has two heat release peaks, which is also caused by the two components. Its maximum heat release peak is higher, indicating a higher fire hazard. The heat release peak of the modified polyester / cotton blended fabric is significantly lower, indicating a lower fire hazard.
[0067] In summary, the present invention synthesizes a multifunctional modifier containing an aromatic group, a phosphate radical and a Schiff base structure by allowing the amino groups of p-phenylenediamine and aniline to undergo a Schiff base reaction with the aldehyde group of p-terephthalaldehyde, and the PH bond of phosphorous acid and DOPO to undergo a Pudovik addition reaction with the Schiff base C=N structure; (1) first, the multifunctional modifier contains an aromatic structure and has a large affinity with polyester fibers. During the high-temperature baking process, the instantaneous gaps in the polyester fibers are opened, and the multifunctional modifier molecules can diffuse into the interior of the polyester fibers and combine with the polyester fibers through the principle of like dissolves like; (2) in addition, the ammonium phosphate structure in the multifunctional modifier molecules undergoes a covalent grafting reaction with the active hydroxyl groups of the cotton fibers under the catalysis of dicyandiamide, so that the flame retardant can be firmly fixed on the polyester fibers and cotton fibers, thereby providing durable flame retardant and antibacterial functions. The phosphorus-containing flame retardant groups, Schiff base C=N structures, and aromatic benzene rings in the flame retardant molecules produce a synergistic flame retardant effect, effectively promoting the charring of polyester / cotton blended fabrics and achieving high flame retardant efficiency. Furthermore, the Schiff base structure exhibits high bioactivity, imparting excellent antibacterial properties to the modified polyester / cotton blended fabric.
[0068] It should be noted that any changes made by those skilled in the art to the specific embodiments of the present invention do not depart from the scope of the claims of the present invention. Accordingly, the scope of the claims of the present invention is not limited to the aforementioned specific embodiments.
Claims
1. A method for preparing a durable flame-retardant, antibacterial, multifunctional modified polyester / cotton blended fabric, characterized in that: It includes the following steps: S1. Aniline and terephthalaldehyde are dissolved in ethanol and reacted at 80-90°C for 3-4 hours. P-phenylenediamine, phosphorous acid and DOPO are added in sequence and the reaction is continued for 5-7 hours. After the reaction, the mixture is subjected to reduced pressure distillation and washing to obtain a multifunctional modifier containing an aromatic group, a phosphate group and a Schiff base structure. S2. Add the multifunctional modifier, ammonia water, dicyandiamide, dispersant NNO and penetrant JFC into the aqueous solution and disperse them for 2 to 3 hours using a high-speed shear emulsifier to prepare a flame retardant dispersion. S3. Using flame retardant dispersion, polyester / cotton blended fabric is treated by dipping-baking method to prepare durable flame retardant and antibacterial multifunctional polyester / cotton blended fabric.
2. The preparation method according to claim 1, characterized in that In step S1, the molar ratio of aniline to terephthalaldehyde is 1:1.2-1.3, the mass ratio of terephthalaldehyde to ethanol is 1:30-50, the molar ratio of p-phenylenediamine to terephthalaldehyde is 1-1.2:2, the molar ratio of phosphorous acid to terephthalaldehyde is 1-1.2:1, and the molar ratio of DOPO to terephthalaldehyde is 1-1.2:
1.
3. The preparation method according to claim 1, characterized in that In step S2, the rotation speed of the high-speed shear emulsifier is 3000-5000 rpm.
4. The preparation method according to claim 1, characterized in that In step S2, the concentration of the multifunctional modifier is 200-300 g / L, the amount of the dispersant NNO is 4-6% of the mass of the flame retardant dispersion, the amount of the penetrant JFC is 3-5 g / L, and the amount of dicyandiamide is 40-60 g / L; The pH value of the flame retardant dispersion is 6-8.
5. The preparation method according to claim 1, characterized in that Step S3 specifically includes the following steps: S31, immersing the polyester / cotton blended fabric in the flame retardant dispersion for padding, wherein the liquid carrying rate of the polyester / cotton blended fabric after padding is 90-110%; S32, pre-baking and baking the padded polyester / cotton blended fabric in sequence, wherein the pre-baking temperature is 70-90° C. for 1-2 min, and the baking temperature is 180-200° C. for 2-4 min.
6. The preparation method according to claim 1, characterized in that In step S3, the polyester / cotton blended fabric is a polyester / cotton blended fabric with a ratio of 40 / 60, 45 / 55, 65 / 35 or 80 / 20.
Citation Information
Patent Citations
DOPO (9,10-dihydID-9-oxa-10-phosphaphenanthrene-10-oxide)-derived phosphorus-nitrogen flame retardant as well as preparation method and application thereof
CN103881134A
Preparation method of durable flame-retardant polyester / cotton blended fabric
CN116623429A
Phosphorus-nitrogen-containing DOPO derivative as well as preparation method and application thereof
CN116655696A