A method for preparing flame-retardant dyed wool-polyester fabric
By synthesizing multifunctional modifiers and chemically react with phosphite, modifying wool-polyester fabrics, and dyeing them with dispersed dyes, the problems of dyeing and flame retardant treatment of wool-polyester-blend textiles are solved, achieving efficient dyeing and flame retardant effects, and the fabric has good water-resistant performance.
Patent Information
- Application Number
- CN202411435037.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-15
- Publication Date
- 2025-03-07
- Estimated Expiration
- 2044-10-15
AI Technical Summary
The dyeing and flame retardant treatment of wool-polyester-blend textiles is technically difficult. Traditional methods require multiple steps to organize, resulting in greater damage to the fabric and poor flame retardant performance.
Design and synthesize multifunctional modifiers, chemically react with phosphite and wool fabrics, form modified wool fabrics, and then dye them with dispersed dyes to achieve flame retardant dyes.
It improves the dyeing rate and color fastness of dye on wool fibers, enhances the flame retardant performance of the fabric, and has excellent water-resistant performance, meeting the B1 standard.
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Figure CN118932748B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of flame retardancy, and in particular relates to a method for preparing a flame retardant dyed wool-polyester fabric. Background Art
[0002] Wool-polyester blended fabric is a kind of fabric carefully woven from wool and polyester blended yarn. It combines the respective advantages of wool and polyester, maintaining the warmth and softness of wool while giving full play to the advantages of polyester in terms of wear resistance, wrinkle resistance, quick drying and easy washing. This kind of fabric is widely used in interior decoration, high-quality bedding and fashion clothing due to its diversified characteristics. However, the dyeing process of wool-polyester blended fabric faces considerable challenges. The reason is that there are essential differences between wool and polyester in fiber structure and performance, which makes the coloring efficiency of traditional disperse dyes on wool low, and reactive dyes or other special dyes are often required for targeted dyeing, which increases the technical difficulty and complexity of dyeing.
[0003] In addition, flame retardant treatment of wool-polyester blended fabrics is also a complex and important issue. When wool burns, it forms a carbonized layer with heat insulation effect, which helps to slow down the spread of fire; while polyester will melt at high temperature and may drip, increasing the risk of fire spread. Therefore, when flame retardant treatment is applied to wool-polyester blended materials, the different combustion characteristics of the two fibers must be fully considered, and comprehensive measures must be taken to ensure the safety performance of the materials.
[0004] References (Zhang Xufeng, Wang Ranran, Liu Yujian, et al. Process selection for dyeing wool-polyester blended fabrics [J]. Dyeing and Finishing Technology, 2019, 41(12): 37-42.) Through a large number of experiments on dyeing wool-polyester blended fabrics with disperse dyes and acid dyes, Anoklon and Anosate dyes with less damage to wool, less staining and better lifting properties were screened out. However, they only work well when used in specific dye combinations, and their use has limitations; References (Zheng Qingkang, Yang Xiaoming, Du Qian. One-bath dyeing of polyester-cotton and wool-polyester blended fabrics with disperse dyes [J]. Printing and Dyeing Auxiliary Agents, 2002, 19(6): 14-16, 23.) Auxiliary agents with aromatic conjugated structures and reactive functional groups were synthesized. Adding these auxiliaries to the disperse dye bath can improve the dyeing rate of wool-polyester fabrics dyed with disperse dyes in one bath.
[0005] In addition, wool-polyester fabrics have poor flame retardancy and a "bracket effect", which makes it relatively difficult to flame retardant. Chinese invention patent CN104757721A discloses an anti-static, flame-retardant, oil-proof and water-repellent wool-polyester blended fabric and its preparation method. The anti-static, flame-retardant, oil-proof and water-repellent wool-polyester blended fabric is prepared through weaving-dyeing-flame-retardant finishing-oil-proof and water-repellent finishing. The dyeing and flame-retardant finishing processes are multi-step finishing, which causes great damage to the wool-polyester fabric.
[0006] Therefore, it is of great theoretical significance and practical application value to study a functional modifier that can react with wool fibers, polyester fibers, and disperse dyes to solve the problem of dyeing and flame retardant in the same bath. Summary of the invention
[0007] The purpose of the invention is to solve the problems existing in the prior art and provide a method for preparing a flame retardant dyed wool-polyester fabric.
[0008] To achieve the above object, the scheme adopted by the present invention is as follows:
[0009] A method for preparing a flame retardant dyed wool-polyester fabric comprises the following steps:
[0010] (1) Prepare a multifunctional modifier, the structural formula of which is as follows:
[0011] ;
[0012] (2) The wool-polyester fabric is modified by using a multifunctional modifier and a phosphite, and a chemical reaction is controlled between the multifunctional modifier, the phosphite and the wool fiber in the wool-polyester fabric to obtain a modified wool-polyester fabric;
[0013] (3) The modified wool-polyester fabric is dyed with disperse dye solution to obtain flame-retardant dyed wool-polyester fabric.
[0014] As the preferred technical solution:
[0015] The method for preparing a flame retardant dyed wool-polyester fabric as described above, the process of step (1) is: Figure 1 The synthetic route of the multifunctional modifier shown is specifically to dissolve phosphorus oxychloride and pentaerythritol in solvent a (chloroform), react at 25-30°C for 3-4 hours, add hydroxybenzaldehyde, react at 30-35°C for 2-3 hours, and perform post-treatment (purification by reduced pressure distillation) to obtain a multifunctional modifier, wherein the molar ratio of phosphorus oxychloride, pentaerythritol, and hydroxybenzaldehyde is 2-2.2:1:2;
[0016] The hydrogen nuclear magnetic resonance spectrum of the prepared multifunctional modifier is as follows: Figure 2 As shown, the chemical shifts at 7.5 and 6.8 ppm in the H NMR spectrum are caused by the hydrogen elements in the benzene ring, the chemical shift at 9.8 ppm is caused by the hydrogen elements in the aldehyde group, and the chemical shift at 3.8 ppm is caused by the hydrogen elements in the cyclic phosphate pentaerythritol structure. The results show that the multifunctional modifier is successfully synthesized.
[0017] In the method for preparing a flame-retardant dyed wool-polyester fabric as described above, the hydroxybenzaldehyde is one or more of p-hydroxybenzaldehyde, m-hydroxybenzaldehyde, and vanillin; the mass ratio of phosphorus oxychloride to solvent a is 1:30-40, and an increase in the amount of solvent a helps promote uniform reaction, but too high an amount is wasteful.
[0018] In the method for preparing a flame retardant dyed wool-polyester fabric as described above, the specific process of step (2) is: adding a multifunctional modifier, a phosphite and a wool-polyester fabric into a solvent b, reacting at 85-95° C. for 40-70 min, and performing post-treatment to obtain a modified wool-polyester fabric.
[0019] At a higher reaction temperature, the wool scale layer opens, and the multifunctional modifier and phosphite enter the wool fiber. Wool fibers are rich in active amino and hydroxyl groups, which can react with the aldehyde group of the multifunctional modifier and the PH bond of the phosphite to form a Mannich reaction, thereby grafting the multifunctional modifier and phosphite onto the wool fiber through covalent bonds. The multifunctional modifier is rich in aromatic conjugated benzene ring structures and six-membered ring structures, and has a high affinity with polyester fibers. It is combined through the principle of similar phase dissolution, so the multifunctional modifier has a good combination with wool-polyester fabrics.
[0020] According to the method for preparing a flame-retardant dyed wool-polyester fabric, the ratio of the multifunctional modifier to the solvent b is 20-40 g:1 L, the mass ratio of the wool-polyester fabric to the solvent b is 1:30-40, the molar ratio of the multifunctional modifier to the phosphite is 1:2-2.2; the phosphite is one or more of diethyl phosphite or dimethyl phosphite; and the content of wool fiber in the wool-polyester fabric is 40-80 wt%.
[0021] In the method for preparing a flame-retardant dyed wool-polyester fabric as described above, in step (3), the components and contents in the disperse dye solution are as follows: disperse dye 1-2% owf, dispersant (NNO) 0.3-0.5 g / L, carrier (methyl salicylate, during the dyeing process, the carrier can promote the swelling and plasticization of polyester fibers, and can lower the glass transition temperature, open the pores for the dye to enter the fiber, and realize low-temperature dyeing treatment) 1.0-2.0 g / L, acetic acid, water; the pH value of the disperse dye solution is 4-5; the dyeing temperature is 95-98°C, the dyeing time is 50-80 min, and the bath ratio is 1:30-40.
[0022] According to the method for preparing a flame-retardant dyed wool-polyester fabric, the flame-retardant dyed wool-polyester fabric has a dry friction fastness of more than level 4, a wet friction fastness of more than level 3-4, a color change fastness of more than level 4, a staining fastness of more than level 3-4, and a high color yield and color fastness of disperse dye dyeing. Because the multifunctional modifier is rich in aromatic benzene ring structure, it can increase the van der Waals force, hydrogen bond force and π-π bond between the disperse dye and the wool fiber, which is helpful to improve the dyeing rate and color fastness of the disperse dye on the wool fiber. degree, limiting oxygen index ≥28.1%, damaged length ≤9.8cm, with excellent flame retardant properties, because the phosphate structure of phosphite and cyclic phosphate in the flame retardant dyed wool-polyester fabric acts as an acid source, and the aromatic structure containing hydroxybenzaldehyde acts as a carbon source, with high flame retardant efficiency. After 30 washes, the damaged length is still ≤14.7cm, meeting the B1 grade standard, and has excellent water wash resistance, because the flame retardant modifier not only produces covalent bonds with wool fibers, but also has a strong bonding ability with polyester fibers. Beneficial Effects
[0023] The multifunctional modifier and phosphite designed and synthesized by the present invention enter the interior of the wool fiber, and the active amino group and hydroxyl group rich in the wool fiber can react with the aldehyde group of the multifunctional modifier and the PH bond of the phosphite to graft the multifunctional modifier and the phosphite on the wool fiber through covalent bonds. The multifunctional modifier is rich in aromatic conjugated benzene ring structures and six-membered ring structures, has a high affinity with polyester fibers, and is combined through the principle of similar phase dissolution, so that the multifunctional modifier and the wool-polyester fabric have good combination;
[0024] The multifunctional modifier designed and synthesized by the present invention is rich in aromatic benzene ring structure, which can increase the van der Waals force, hydrogen bond force and π-π bond effect between the disperse dye and the wool fiber, thereby improving the dyeing rate and color fastness of the disperse dye on the wool fiber;
[0025] In the flame-retardant dyed wool-polyester fabric of the present invention, the phosphate structures of phosphite and cyclic phosphate serve as acid sources, and the aromatic structure containing hydroxybenzaldehyde serves as a carbon source, and the flame-retardant efficiency is high. At the same time, the flame-retardant modifier not only forms a covalent bond with the wool fiber, but also has a strong bonding ability with the polyester fiber, so that the flame-retardant dyed wool-polyester fabric has excellent water-resistant performance. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] Figure 1 Schematic diagram of the synthesis route of the multifunctional modifier of the present invention;
[0027] Figure 2 It is the hydrogen nuclear magnetic resonance spectrum of the multifunctional modifier of the present invention. DETAILED DESCRIPTION
[0028] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.
[0029] The structural formula of the multifunctional modifier prepared in the embodiment is:
[0030] .
[0031] The following are the methods for testing the relevant performance indicators in the embodiments and comparative examples:
[0032] Dry rubbing fastness and wet rubbing fastness: Tested in accordance with GB / T 3920-2008 Textiles - Tests for colour fastness - Colour fastness to rubbing;
[0033] Color fastness and staining fastness: Tested in accordance with GB / T 3921-2008 Textiles - Tests for color fastness - Color fastness to washing with soap;
[0034] Limiting oxygen index: Tested in accordance with GB / T 5454-1997 "Oxygen Index Method for Textile Combustion Performance Test".
[0035] Damage length: measured in accordance with GB / T 5455-2014 "Determination of smoldering and afterflaming time of damage length in vertical direction of burning performance of textiles".
[0036] Damaged length after 30 washes: First wash the fabric 30 times with water according to AATCC 61-2013 "Accelerated test for color fastness to household and commercial washing" standard, and then test the damaged length of the fabric with reference to GB / T 5455-2014 "Determination of damage length in vertical direction, smoldering and afterflaming time of textile combustion performance" standard.
[0037] Example 1
[0038] A method for preparing a flame retardant dyed wool-polyester fabric, the specific steps are as follows:
[0039] (1) Raw material preparation:
[0040] Wool-polyester fabric: The wool fiber content is 40wt%;
[0041] Phosphorus oxychloride;
[0042] Pentaerythritol;
[0043] Solvent a: chloroform;
[0044] Containing hydroxybenzaldehyde: p-hydroxybenzaldehyde;
[0045] Phosphite: diethyl phosphite;
[0046] Solvent b: ethanol aqueous solution, ethanol accounts for 15% of the total volume;
[0047] Disperse dye solution: pH value is 4, components and contents are: disperse dye (disperse blue 2BLN) 1% owf, dispersant (NNO) 0.3g / L, carrier (methyl salicylate) 1g / L, acetic acid, water;
[0048] (2) Preparation of multifunctional modifier:
[0049] Phosphorus oxychloride and pentaerythritol are dissolved in solvent a, reacted at 25°C for 4 hours, hydroxybenzaldehyde is added, reacted at 30°C for 3 hours, and purified by reduced pressure distillation to obtain a multifunctional modifier;
[0050] Wherein, the mass ratio of phosphorus oxychloride to solvent a is 1:30, and the molar ratio of phosphorus oxychloride, pentaerythritol, and hydroxybenzaldehyde is 2:1:2;
[0051] (3) Modification of wool-polyester fabrics:
[0052] Adding a multifunctional modifier, phosphite and wool-polyester fabric into solvent b, reacting at 85° C. for 70 minutes, and performing post-treatment to obtain a modified wool-polyester fabric;
[0053] The ratio of the multifunctional modifier to the solvent b is 20 g:1 L, the mass ratio of the wool-polyester fabric to the solvent b is 1:40, and the molar ratio of the multifunctional modifier to the phosphite is 1:2;
[0054] (4) Preparation of flame-retardant dyed wool-polyester fabrics:
[0055] The modified wool-polyester fabric was dyed with disperse dye liquor to obtain flame-retardant dyed wool-polyester fabric; wherein the dyeing temperature was 95°C, the dyeing time was 80 min, and the bath ratio was 1:30.
[0056] The final flame-retardant dyed wool-polyester fabric has a dry rubbing fastness of 4-5, a wet rubbing fastness of 4, a color fastness of 4-5, a staining fastness of 4, a limiting oxygen index of 28.1%, a damaged length of 9.8 cm, and a damaged length of 14.7 cm after 30 washes.
[0057] Comparative Example 1
[0058] A method for preparing a flame retardant dyed wool-polyester fabric is basically the same as in Example 1, and the specific steps are as follows:
[0059] (1) Raw material preparation:
[0060] Methanol was added to the raw materials in step (1) of Example 1, and the other raw materials remained unchanged;
[0061] (2) Preparation of multifunctional modifier:
[0062] Phosphorus oxychloride and pentaerythritol are dissolved in solvent a, reacted at 25°C for 4 hours, hydroxybenzaldehyde and methanol are added, reacted at 30°C for 3 hours, and purified by reduced pressure distillation to obtain a multifunctional modifier;
[0063] Wherein, the mass ratio of phosphorus oxychloride to solvent a is 1:30, and the molar ratio of phosphorus oxychloride, pentaerythritol, hydroxybenzaldehyde, and methanol is 2:1:1:1;
[0064] (3) Modification of wool-polyester fabrics:
[0065] Same as step (3) in Example 1;
[0066] (4) Preparation of flame-retardant dyed wool-polyester fabrics:
[0067] Same as step (4) of Example 1.
[0068] The final flame-retardant dyed wool-polyester fabric has a dry rubbing fastness of 3-4, a wet rubbing fastness of 3, a color fastness of 3-4, a staining fastness of 3, a limiting oxygen index of 27.9%, a damaged length of 10.5 cm, and a damaged length of 21.5 cm after 30 washes.
[0069] It can be seen from the data of Example 1 and Comparative Example 1 that the friction fastness, color fastness and flame retardant water washing resistance of the flame retardant dyed wool-polyester fabric prepared in Comparative Example 1 are all reduced. This is because the multifunctional modifier prepared in Comparative Example 1 contains only one aldehyde group. When modifying the wool-polyester fabric, the cross-linking efficiency between the multifunctional modifier and the wool fiber is reduced, and hydrolysis occurs during the washing process, resulting in reduced color fastness and flame retardant properties during the washing process.
[0070] Comparative Example 2
[0071] A method for preparing a flame retardant dyed wool-polyester fabric is basically the same as in Example 1, and the specific steps are as follows:
[0072] (1) Raw material preparation:
[0073] The hydroxybenzaldehyde in step (1) of Example 1 was replaced by glyceraldehyde, and the other raw materials remained unchanged;
[0074] (2) Preparation of multifunctional modifier:
[0075] Phosphorus oxychloride and pentaerythritol are dissolved in solvent a, reacted at 25°C for 4 hours, glyceraldehyde is added, reacted at 30°C for 3 hours, and purified by reduced pressure distillation to obtain a multifunctional modifier;
[0076] Wherein, the mass ratio of phosphorus oxychloride to solvent a is 1:30, and the molar ratio of phosphorus oxychloride, pentaerythritol, and glyceraldehyde is 2:1:2;
[0077] (3) Modification of wool-polyester fabrics:
[0078] Same as step (3) in Example 1;
[0079] (4) Preparation of flame-retardant dyed wool-polyester fabrics:
[0080] Same as step (4) of Example 1.
[0081] The final flame-retardant dyed wool-polyester fabric has a dry rubbing fastness of level 3, a wet rubbing fastness of level 2-3, a color fastness of level 3, a staining fastness of level 3, a limiting oxygen index of 27.5%, a damaged length of 10.7 cm, and a damaged length of 30 cm after 30 washes.
[0082] It can be seen from the data of Example 1 and Comparative Example 2 that the friction fastness, color fastness and flame retardant water washing resistance of the flame retardant dyed wool-polyester fabric prepared in Comparative Example 2 are significantly reduced. This is because the multifunctional modifier prepared in Comparative Example 2 does not contain an aromatic structure. The aromatic benzene ring structure can increase the van der Waals force, hydrogen bonding force and π-π bonding between the disperse dye and the wool fiber, which helps to improve the dyeing rate and color fastness of the disperse dye on the wool fiber. At the same time, the aromatic conjugated benzene ring structure has a high affinity with the polyester fiber, and is combined with the wool-polyester fabric through the principle of similar phase dissolution, and has a good combination with the wool-polyester fabric. However, the multifunctional modifier prepared in Comparative Example 2 lacks this aromatic benzene ring structure, so the friction fastness, color fastness and flame retardant water washing resistance of the flame retardant dyed wool-polyester fabric prepared in Comparative Example 2 are low.
[0083] Comparative Example 3
[0084] A method for dyeing wool-polyester fabrics comprises using disperse dye liquor (the same as in Example 1) to finish the wool-polyester fabrics (the method and process parameters are the same as in Example 1) to obtain dyed wool-polyester fabrics.
[0085] The final dyed wool-polyester fabric has a dry rubbing fastness of 2-3, a wet rubbing fastness of 2, a color fastness of 2-3, a staining fastness of 2-3, a limiting oxygen index of 20.6%, a damaged length of 30 cm, and a damaged length of 30 cm after 30 washes.
[0086] Example 2
[0087] A method for preparing a flame retardant dyed wool-polyester fabric, the specific steps are as follows:
[0088] (1) Raw material preparation:
[0089] Wool-polyester fabric: The wool fiber content is 45wt%;
[0090] Phosphorus oxychloride;
[0091] Pentaerythritol;
[0092] Solvent a: chloroform;
[0093] Containing hydroxybenzaldehyde: m-hydroxybenzaldehyde;
[0094] Phosphite: dimethyl phosphite;
[0095] Solvent b: ethanol-water solution, ethanol accounts for 16% of the total volume;
[0096] Disperse dye solution: pH value is 4.5, components and contents are: disperse dye (disperse blue 2BLN) 1.3% owf, dispersant (NNO) 0.4 g / L, carrier (methyl salicylate) 1.5 g / L, acetic acid, water;
[0097] (2) Preparation of multifunctional modifier:
[0098] Phosphorus oxychloride and pentaerythritol are dissolved in solvent a, reacted at 27°C for 3.7 hours, hydroxybenzaldehyde is added, reacted at 31°C for 2.7 hours, and purified by reduced pressure distillation to obtain a multifunctional modifier;
[0099] Wherein, the mass ratio of phosphorus oxychloride to solvent a is 1:35, and the molar ratio of phosphorus oxychloride, pentaerythritol, and hydroxybenzaldehyde is 2.1:1:2;
[0100] (3) Modification of wool-polyester fabrics:
[0101] Adding a multifunctional modifier, phosphite and wool-polyester fabric into solvent b, reacting at 89° C. for 60 min, and performing post-treatment to obtain a modified wool-polyester fabric;
[0102] Among them, the ratio of the multifunctional modifier to the solvent b is 25g:1L, the mass ratio of the wool-polyester fabric to the solvent b is 1:35, and the molar ratio of the multifunctional modifier to the phosphite is 1:2.1;
[0103] (4) Preparation of flame-retardant dyed wool-polyester fabrics:
[0104] The modified wool-polyester fabric was dyed with disperse dye liquor to obtain flame-retardant dyed wool-polyester fabric; wherein the dyeing temperature was 96°C, the dyeing time was 60 min, and the bath ratio was 1:35.
[0105] The final flame-retardant dyed wool-polyester fabric has a dry rubbing fastness of 4-5, a wet rubbing fastness of 4, a color fastness of 4-5, a staining fastness of 4, a limiting oxygen index of 29.7%, a damaged length of 9.1 cm, and a damaged length of 14.1 cm after 30 washes.
[0106] Comparative Example 4
[0107] A method for dyeing wool-polyester fabric, comprising: using disperse dye liquor (the same as in Example 2) to finish the wool-polyester fabric (the method and process parameters are the same as in Example 2) to obtain the dyed wool-polyester fabric.
[0108] The final dyed wool-polyester fabric has a dry rubbing fastness of 2-3, a wet rubbing fastness of 2, a color change fastness of 2-3, a staining fastness of 2-3, a limiting oxygen index of 20.8%, a damaged length of 30 cm, and a damaged length of 30 cm after 30 washes.
[0109] Example 3
[0110] A method for preparing a flame retardant dyed wool-polyester fabric, the specific steps are as follows:
[0111] (1) Raw material preparation:
[0112] Wool-polyester fabric: The wool fiber content is 65wt%;
[0113] Phosphorus oxychloride;
[0114] Pentaerythritol;
[0115] Solvent a: chloroform;
[0116] Contains hydroxybenzaldehyde: vanillin;
[0117] Phosphite: diethyl phosphite;
[0118] Solvent b: ethanol aqueous solution, ethanol accounts for 18% of the total volume;
[0119] Disperse dye solution: pH value is 4.5, components and contents are: disperse dye (disperse blue 2BLN) 1.6% owf, dispersant (NNO) 0.45 g / L, carrier (methyl salicylate) 1.7 g / L, acetic acid, water;
[0120] (2) Preparation of multifunctional modifier:
[0121] Phosphorus oxychloride and pentaerythritol are dissolved in solvent a, reacted at 29°C for 3.4 hours, hydroxybenzaldehyde is added, reacted at 33°C for 2.4 hours, and purified by reduced pressure distillation to obtain a multifunctional modifier;
[0122] Wherein, the mass ratio of phosphorus oxychloride to solvent a is 1:40, and the molar ratio of phosphorus oxychloride, pentaerythritol, and hydroxybenzaldehyde is 2.2:1:2;
[0123] (3) Modification of wool-polyester fabrics:
[0124] Adding a multifunctional modifier, phosphite and wool-polyester fabric into solvent b, reacting at 93° C. for 50 min, and performing post-treatment to obtain a modified wool-polyester fabric;
[0125] Among them, the ratio of the multifunctional modifier to the solvent b is 30 g:1 L, the mass ratio of the wool-polyester fabric to the solvent b is 1:35, and the molar ratio of the multifunctional modifier to the phosphite is 1:2.2;
[0126] (4) Preparation of flame-retardant dyed wool-polyester fabrics:
[0127] The modified wool-polyester fabric was dyed with disperse dye liquor to obtain flame-retardant dyed wool-polyester fabric; wherein the dyeing temperature was 97°C, the dyeing time was 70 min, and the bath ratio was 1:40.
[0128] The final flame-retardant dyed wool-polyester fabric has a dry rubbing fastness of level 4, a wet rubbing fastness of level 4, a color fastness of level 4, a staining fastness of level 4, a limiting oxygen index of 30.9%, a damaged length of 8.5 cm, and a damaged length of 13.5 cm after 30 washes.
[0129] Comparative Example 5
[0130] A method for dyeing wool-polyester fabric, comprising: using disperse dye liquor (the same as in Example 3) to finish the wool-polyester fabric (the method and process parameters are the same as in Example 3) to obtain the dyed wool-polyester fabric.
[0131] The final dyed wool-polyester fabric has a dry rubbing fastness of 2-3, a wet rubbing fastness of 2, a color fastness of 2-3, a staining fastness of 2-3, a limiting oxygen index of 20.9%, a damaged length of 30 cm, and a damaged length of 30 cm after 30 washes.
[0132] Example 4
[0133] A method for preparing a flame retardant dyed wool-polyester fabric, the specific steps are as follows:
[0134] (1) Raw material preparation:
[0135] Wool-polyester fabric: The wool fiber content is 80wt%;
[0136] Phosphorus oxychloride;
[0137] Pentaerythritol;
[0138] Solvent a: chloroform;
[0139] Hydroxybenzaldehyde-containing: a mixture of p-hydroxybenzaldehyde and m-hydroxybenzaldehyde in a mass ratio of 1:1;
[0140] Phosphite: dimethyl phosphite;
[0141] Solvent b: ethanol aqueous solution, ethanol accounts for 20% of the total volume;
[0142] Disperse dye solution: pH value is 5, components and contents are: disperse dye (disperse blue 2BLN) 2% owf, dispersant (NNO) 0.5 g / L, carrier (methyl salicylate) 2 g / L, acetic acid, water;
[0143] (2) Preparation of multifunctional modifier:
[0144] Phosphorus oxychloride and pentaerythritol are dissolved in solvent a, reacted at 30°C for 3 hours, hydroxybenzaldehyde is added, reacted at 35°C for 2 hours, and purified by reduced pressure distillation to obtain a multifunctional modifier;
[0145] Wherein, the mass ratio of phosphorus oxychloride to solvent a is 1:35, and the molar ratio of phosphorus oxychloride, pentaerythritol, and hydroxybenzaldehyde is 2.1:1:2;
[0146] (3) Modification of wool-polyester fabrics:
[0147] Adding a multifunctional modifier, phosphite and wool-polyester fabric into solvent b, reacting at 95° C. for 40 minutes, and performing post-treatment to obtain a modified wool-polyester fabric;
[0148] Among them, the ratio of the multifunctional modifier to the solvent b is 40g:1L, the mass ratio of the wool-polyester fabric to the solvent b is 1:30, and the molar ratio of the multifunctional modifier to the phosphite is 1:2.2;
[0149] (4) Preparation of flame-retardant dyed wool-polyester fabrics:
[0150] The modified wool-polyester fabric was dyed with disperse dye liquor to obtain flame-retardant dyed wool-polyester fabric; wherein the dyeing temperature was 98°C, the dyeing time was 50 min, and the bath ratio was 1:35.
[0151] The final flame-retardant dyed wool-polyester fabric has a dry rubbing fastness of level 4, a wet rubbing fastness of level 3-4, a color fastness of level 4, a staining fastness of level 3-4, a limiting oxygen index of 31.5%, a damaged length of 8.1 cm, and a damaged length of 12.9 cm after 30 washes.
[0152] Comparative Example 6
[0153] A method for dyeing wool-polyester fabric, comprising: using disperse dye liquor (the same as in Example 4) to finish the wool-polyester fabric (the method and process parameters are the same as in Example 4) to obtain the dyed wool-polyester fabric.
[0154] The final dyed wool-polyester fabric has a dry rubbing fastness of 2-3, a wet rubbing fastness of 2, a color fastness of 2-3, a staining fastness of 2-3, a limiting oxygen index of 21%, a damaged length of 30 cm, and a damaged length of 30 cm after 30 washes.
Claims
1. A method for preparing a flame retardant dyed wool-polyester fabric, characterized in that: The following steps are involved: (1) Prepare a multifunctional modifier, the structural formula of the multifunctional modifier is as follows: (2) using a multifunctional modifier and a phosphite to modify the wool-polyester fabric, controlling a chemical reaction between the multifunctional modifier, the phosphite and the wool fibers in the wool-polyester fabric, and obtaining a modified wool-polyester fabric; (3) The modified wool-polyester fabric is dyed with disperse dye solution to obtain flame-retardant dyed wool-polyester fabric.
2. The method for preparing a flame retardant dyed wool-polyester fabric according to claim 1, characterized in that: The process of step (1) is as follows: phosphorus oxychloride and pentaerythritol are dissolved in solvent a, reacted at 25-30° C. for 3-4 hours, hydroxybenzaldehyde is added, reacted at 30-35° C. for 2-3 hours, and post-treated to obtain a multifunctional modifier, wherein the molar ratio of phosphorus oxychloride, pentaerythritol, and hydroxybenzaldehyde is 2-2.2:1:
2.
3. The method for preparing a flame retardant dyed wool-polyester fabric according to claim 2, characterized in that: The hydroxybenzaldehyde is p-hydroxybenzaldehyde.
4. The method for preparing a flame retardant dyed wool-polyester fabric according to claim 1, characterized in that: The specific process of step (2) is: adding the multifunctional modifier, phosphite and wool-polyester fabric into solvent b, reacting at 85-95° C. for 40-70 minutes, and performing post-treatment to obtain the modified wool-polyester fabric.
5. The method for preparing a flame retardant dyed wool-polyester fabric according to claim 4, characterized in that: The ratio of the multifunctional modifier to the solvent b is 20-40 g:1 L, the mass ratio of the wool-polyester fabric to the solvent b is 1:30-40, and the molar ratio of the multifunctional modifier to the phosphite is 1:2-2.2; the phosphite is one or more of diethyl phosphite or dimethyl phosphite; The wool fiber content in the wool-polyester fabric is 40-80wt%.
6. The method for preparing a flame retardant dyed wool-polyester fabric according to claim 1, characterized in that: In step (3), the components and contents in the disperse dye solution are as follows: disperse dye 1-2% owf, dispersant 0.3-0.5 g / L, carrier 1.0-2.0 g / L, acetic acid, water; the pH value of the disperse dye solution is 4-5; the dyeing temperature is 95-98° C., the dyeing time is 50-80 min, and the bath ratio is 1:30-40.
7. The method for preparing a flame retardant dyed wool-polyester fabric according to claim 1, characterized in that: The dry rubbing fastness of flame retardant dyed wool-polyester fabric is above grade 4, the wet rubbing fastness is above grade 3-4, the color fastness is above grade 4, the staining fastness is above grade 3-4, the limiting oxygen index is ≥28.1%, the damaged length is ≤9.8cm, and the damaged length is still ≤14.7cm after 30 washes.
Citation Information
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