A clothing fabric, its preparation method and application

Abstract

The present invention belongs to the field of fabric technology, specifically relating to a clothing fabric, its preparation method, and its application. The preparation method comprises the following steps: blending KH-602-modified zinc cerium phenylphosphonate, SA-DOPO flame retardant, and polylactic acid particles at a certain temperature, followed by spinning to produce polylactic acid fibers; and then spinning and weaving the polylactic acid fibers to produce clothing fabric. By adding KH-602-modified zinc cerium phenylphosphonate and SA-DOPO flame retardant, the present invention utilizes the interaction between the components to jointly enhance the flame retardant properties of the fabric, making it well-suited for use in protective clothing.

Description

Technical Field

[0001] The present invention belongs to the technical field of fabrics, and more specifically, relates to a clothing fabric, a preparation method thereof, and an application thereof. Background Art

[0002] Polylactic acid (PLA) fiber is derived from raw materials such as corn and wheat. It uses no petroleum and exhibits excellent biodegradability, biocompatibility, and bioabsorbability. It combines the excellent mechanical properties of both synthetic and natural fibers, attracting increasing attention as a sustainable and eco-friendly fiber. However, PLA fabrics are flammable, generating significant heat and smoke when burned. These factors can easily fuel fires and cause them to spread, posing serious risks to human production, livelihoods, and even life. This, to a certain extent, has limited the development and widespread application of PLA fabrics.

[0003] CN114921870A discloses a flame-retardant polylactic acid fabric and a method for preparing the same. The fabric is characterized by the following process: first, reacting hydroxyl-terminated polydimethylsiloxane, dimethyl phosphate, and hexachlorocyclotriphosphazene to produce a nitrogen-containing phosphorus-silicon flame retardant; then, blending the nitrogen-containing phosphorus-silicon flame retardant with polylactic acid particles and spinning them to produce polylactic acid fibers; and finally, spinning and weaving the polylactic acid fibers to produce the flame-retardant polylactic acid fabric. The flame-retardant polylactic acid fabric produced by the present invention exhibits an initial limiting oxygen index exceeding 35%, which is within the range of flame-retardant materials; after 10 washes, the limiting oxygen index remains above 32%, with no significant decrease. The flame-retardant polylactic acid fabric produced by the present method exhibits strong flame retardancy, is simple to manufacture, is inexpensive, and has minimal environmental impact.

[0004] CN113151922A discloses a flame-retardant polylactic acid fiber elastic fabric and its preparation method, relating to the field of new materials technology. The method first reacts phloroglucinol with an alkylating agent, and then further reacts sodium lignin sulfonate in the presence of potassium iodide to produce modified lignin. The modified lignin is then mixed with nano-metal powder to produce modified nano-metal. Bacterial cellulose is then reacted with maleic anhydride to produce modified bacterial cellulose. The modified nano-metal is then reacted with epoxidized soybean oil in the presence of a tertiary amine catalyst, and then reacted with the modified bacterial cellulose to produce a modified additive. Finally, the modified additive and plasticizer are added to polyethylene, extruded, and melt-spun to produce a polylactic acid fiber billet. The polylactic acid fiber billet is then hydrothermally carbonized, spun, and woven to produce the flame-retardant polylactic acid fiber elastic fabric. The flame-retardant polylactic acid fiber elastic fabric produced by the present invention exhibits excellent electrical conductivity and flame retardancy, as well as good mechanical properties.

[0005] By co-spinning flame-retardant components with polylactic acid, polylactic acid with flame-retardant properties can be produced. However, the cost of adding the components is high or the components are easily washed away, resulting in a decrease in flame-retardant properties after multiple washings. Summary of the Invention

[0006] The present invention aims to overcome the defects and shortcomings of the prior art by providing a clothing fabric, a preparation method, and its application. The preparation method comprises the following steps: blending KH-602-modified zinc cerium phenylphosphonate, an SA-DOPO flame retardant, and polylactic acid particles at a certain temperature, followed by spinning to produce polylactic acid fibers; and then spinning and weaving the polylactic acid fibers to produce clothing fabric. By adding KH-602-modified zinc cerium phenylphosphonate and an SA-DOPO flame retardant, the present invention utilizes the interaction between the components to enhance the flame retardancy of the fabric, enabling its application in protective clothing.

[0007] The purpose of the present invention is to provide a method for preparing clothing fabrics.

[0008] Another object of the present invention is to provide a clothing fabric.

[0009] Another object of the present invention is to provide an application of clothing fabrics.

[0010] The above-mentioned purpose of the present invention is achieved through the following technical solutions:

[0011] A method for preparing a clothing fabric, comprising the following steps:

[0012] KH-602 modified zinc cerium phenylphosphonate, SA-DOPO flame retardant and polylactic acid particles are blended at a certain temperature, and then spun to obtain polylactic acid fibers; and then the polylactic acid fibers are spun and woven to obtain clothing fabrics.

[0013] Preferably, the blending temperature is 165-175° C.; the mass ratio of the KH-602 modified zinc cerium phenylphosphonate, SA-DOPO flame retardant and polylactic acid particles is 3-5:2-4:400-440.

[0014] In the present invention, the preferred technical solution is that the preparation method of the KH-602 modified cerium zinc phenylphosphonate comprises the following steps:

[0015] The zinc salt, cerium salt and phenylphosphonic acid are ultrasonically dispersed in deionized water, stirred for a certain period of time, and then refluxed and then hydrothermally reacted. The mixture is cooled to room temperature, washed and dried to obtain zinc cerium phenylphosphonate. The obtained zinc cerium phenylphosphonate and KH-602 (N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane) are ultrasonically dispersed in ethanol water, and then stirred and reacted. The mixture is cooled to room temperature, filtered, washed and dried to obtain KH-602-modified zinc cerium phenylphosphonate.

[0016] Preferably, the zinc salt is at least one of zinc nitrate, zinc acetate, and zinc chloride, the cerium salt is at least one of cerium nitrate, cerium acetate, and cerium chloride, and the molar ratio of the zinc salt, cerium salt, and phenylphosphonic acid is: 0.1-0.3:0.7-0.9; 2.

[0017] Preferably, the stirring time is 20 to 40 minutes; the reflux reaction condition is reflux reaction at 85 to 95° C. for 20 to 30 hours; the hydrothermal condition is hydrothermal reaction at 100 to 140° C. for 16 to 24 hours; and the drying is drying at 80 to 100° C. for 10 to 14 hours.

[0018] Preferably, the volume ratio of ethanol to water is 2:1; the mass ratio of cerium zinc phenylphosphonate to KH-602 is 10:0.5-0.9; and the stirring reaction is carried out at 40-60° C. for 2-4 hours.

[0019] In the present invention, the preferred technical solution is that the preparation method of the SA-DOPO flame retardant comprises the following steps:

[0020] Salicylaldehyde (SA) and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were ultrasonically dispersed in DMF, stirred under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and vacuum dried to obtain SA-DOPO.

[0021] Preferably, the molar ratio of SA to DOPO is 1:2.5-3.5; the stirring reaction is carried out at 110-120° C. for 5-7 hours; and the vacuum drying is carried out at 70-90° C. for 12-20 hours.

[0022] A clothing fabric is prepared based on the above-mentioned method for preparing a clothing fabric.

[0023] Based on the application of the above-mentioned clothing fabrics in fire-resistant clothing.

[0024] The present invention has the following beneficial effects:

[0025] By preparing zinc cerium phenylphosphonate and then modifying it with KH-602, its dispersibility in polylactic acid can be improved, and it is not easy to fall off, and the flame retardant properties of the fabric can be improved. SA-DOPO flame retardant is obtained by reacting salicylaldehyde with DOPO. SA-DOPO flame retardant is compounded with KH-602-modified zinc cerium phenylphosphonate to jointly promote the improvement of the flame retardant properties of the fabric. The flame retardant properties are excellent and still have excellent flame retardant properties after multiple washings. DETAILED DESCRIPTION

[0026] The present invention is further described below with reference to specific examples, which, however, are not intended to limit the present invention in any way. Unless otherwise specified, the reagents, methods, and equipment used in the present invention are conventional reagents, methods, and equipment in the art.

[0027] Polylactic acid 4032D265: Dongguan Zhangmutou Hongji Plastics Trading Co., Ltd.

[0028] Unless otherwise specified, the reagents and materials used in the following examples were commercially available.

[0029] Example 1

[0030] A method for preparing a clothing fabric, comprising the following steps:

[0031] 40g KH-602 modified zinc cerium phenylphosphonate, 30g SA-DOPO flame retardant and 4200g polylactic acid particles were blended at 170°C and then spun to obtain polylactic acid fibers; the polylactic acid fibers were then spun and woven to obtain clothing fabrics.

[0032] The preparation method of the KH-602 modified cerium zinc phenylphosphonate comprises the following steps:

[0033] 0.2 mol zinc nitrate, 0.8 mol cerium acetate and 2 mol phenylphosphonic acid were ultrasonically dispersed in 200 mL deionized water, stirred for 30 min, then refluxed at 90 ° C for 26 h, then hydrothermally reacted at 120 ° C for 20 h, cooled to room temperature, washed, and dried at 90 ° C for 12 h to obtain cerium zinc phenylphosphonate; 10 g cerium zinc phenylphosphonate and 0.7 g KH-602 (N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane) were ultrasonically dispersed in ethanol water (the volume ratio of ethanol to water was 2:1), then stirred at 50 ° C for 3 h, cooled to room temperature, filtered, washed, and dried at 90 ° C for 12 h to obtain KH-602-modified cerium zinc phenylphosphonate.

[0034] Preparation method of SA-DOPO flame retardant

[0035] 1 mol of salicylaldehyde (SA) and 3 mol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were ultrasonically dispersed in 150 mL of DMF. The mixture was stirred at 115°C for 6 h under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and dried in vacuo at 80°C for 16 h to obtain SA-DOPO.

[0036] Example 2

[0037] A method for preparing a clothing fabric, comprising the following steps:

[0038] 50g KH-602 modified zinc cerium phenylphosphonate, 20g SA-DOPO flame retardant and 4400g polylactic acid particles were blended at 170°C and then spun to obtain polylactic acid fibers; the polylactic acid fibers were then spun and woven to obtain clothing fabrics.

[0039] The preparation method of the KH-602 modified cerium zinc phenylphosphonate comprises the following steps:

[0040] 0.3 mol zinc acetate, 0.7 mol cerium chloride and 2 mol phenylphosphonic acid were ultrasonically dispersed in 200 mL deionized water, stirred for 40 min, then refluxed at 95 ° C for 20 h, then hydrothermally reacted at 140 ° C for 16 h, cooled to room temperature, washed, and dried at 100 ° C for 10 h to obtain cerium zinc phenylphosphonate; 10 g cerium zinc phenylphosphonate and 0.9 g KH-602 (N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane) were ultrasonically dispersed in 150 mL ethanol water (the volume ratio of ethanol to water was 2:1), then stirred at 60 ° C for 2 h, cooled to room temperature, filtered, washed, and dried at 100 ° C for 10 h to obtain KH-602-modified cerium zinc phenylphosphonate.

[0041] Preparation method of SA-DOPO flame retardant

[0042] 1 mol of salicylaldehyde (SA) and 3.5 mol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were ultrasonically dispersed in 150 mL of DMF. The mixture was stirred at 120°C for 5 h under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and dried in vacuo at 90°C for 12 h to obtain SA-DOPO.

[0043] Example 3

[0044] A method for preparing a clothing fabric, comprising the following steps:

[0045] 30g KH-602 modified zinc cerium phenylphosphonate, 40g SA-DOPO flame retardant and 4000g polylactic acid particles were blended at 170°C and then spun to obtain polylactic acid fibers; the polylactic acid fibers were then spun and woven to obtain clothing fabrics.

[0046] The preparation method of the KH-602 modified cerium zinc phenylphosphonate comprises the following steps:

[0047] 0.1 mol zinc chloride, 0.9 mol cerium nitrate and 2 mol phenylphosphonic acid were ultrasonically dispersed in 200 mL deionized water, stirred for 20 min, then refluxed at 85 ° C for 30 h, then hydrothermally reacted at 100 ° C for 24 h, cooled to room temperature, washed, and dried at 80 ° C for 14 h to obtain cerium zinc phenylphosphonate; 10 g cerium zinc phenylphosphonate and 0.5 g KH-602 (N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane) were ultrasonically dispersed in ethanol water (the volume ratio of ethanol to water was 2:1), then stirred at 40 ° C for 4 h, cooled to room temperature, filtered, washed, and dried at 80 ° C for 14 h to obtain KH-602-modified cerium zinc phenylphosphonate.

[0048] Preparation method of SA-DOPO flame retardant

[0049] 1 mol of salicylaldehyde (SA) and 2.5 mol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were ultrasonically dispersed in DMF. The mixture was stirred at 110°C for 7 h under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and dried in vacuo at 70°C for 20 h to obtain SA-DOPO.

[0050] Comparative Example 1

[0051] Comparative Example 1 is substantially the same as Example 1, except that an equal amount of KH-602-modified cerium phenylphosphonate is used instead of KH-602-modified cerium zinc phenylphosphonate.

[0052] The preparation method of the KH-602 modified cerium phenylphosphonate comprises the following steps:

[0053] 1 mol of cerium acetate and 2 mol of phenylphosphonic acid were ultrasonically dispersed in 200 mL of deionized water, stirred for 30 min, then refluxed at 90 ° C for 26 h, then hydrothermally reacted at 120 ° C for 20 h, cooled to room temperature, washed, and dried at 90 ° C for 12 h to obtain cerium zinc phenylphosphonate; 10 g of cerium phenylphosphonate and 0.7 g of KH-602 (N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane) were ultrasonically dispersed in ethanol water (the volume ratio of ethanol to water was 2:1), then stirred at 50 ° C for 3 h, cooled to room temperature, filtered, washed, and dried at 90 ° C for 12 h to obtain KH-602-modified cerium phenylphosphonate.

[0054] Comparative Example 2

[0055] Comparative Example 2 is substantially the same as Example 1, except that an equal amount of cerium zinc phenylphosphonate is used to replace the KH-602-modified cerium zinc phenylphosphonate.

[0056] The preparation method of the cerium zinc phenylphosphonate comprises the following steps:

[0057] 0.2 mol zinc nitrate, 0.8 mol cerium acetate and 2 mol phenylphosphonic acid were ultrasonically dispersed in 200 mL deionized water, stirred for 30 min, then refluxed at 90 ° C for 26 h, then hydrothermally reacted at 120 ° C for 20 h, cooled to room temperature, washed, and dried at 90 ° C for 12 h to obtain cerium zinc phenylphosphonate.

[0058] Comparative Example 3

[0059] Comparative Example 3 is substantially the same as Example 1, except that the amount of KH-602-modified cerium zinc phenylphosphonate is 70 g, and the SA-DOPO flame retardant is not included.

[0060] The flame retardant properties of Examples 1-3 and Comparative Examples 1-3 were tested. The specific test results are shown in Table 1.

[0061] Among them, the test method adopts the oxygen index test method, that is, according to GB / T 5454-1997 "Textile combustion performance test oxygen index method", refer to GB / T 20944.1-2007 washing fastness test machine washing method to perform standard washing on polylactic acid fabrics.

[0062] Table 1:

[0063]

[0064] As can be seen from Table 1, the clothing fabric prepared according to the present invention has excellent flame retardancy and maintains good flame retardancy even after 15 washes. Specifically, a comparison of Example 1 with Comparative Examples 1-3 shows that the addition of KH-602-modified zinc cerium phenylphosphonate and SA-DOPO flame retardant to the raw materials can significantly improve the flame retardancy of clothing fabrics.

[0065] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be considered as equivalent replacement methods and are included in the scope of protection of the present invention.

Claims

1. A method for preparing a garment fabric, characterized in that: The preparation method comprises the following steps: KH-602 modified zinc cerium phenylphosphonate, SA-DOPO flame retardant and polylactic acid particles are blended at a certain temperature and then spun to produce polylactic acid fibers; the polylactic acid fibers are then spun and woven to produce clothing fabrics; The blending temperature is 165 to 175 ° C; the mass ratio of the KH-602 modified cerium zinc phenylphosphonate, SA-DOPO flame retardant and polylactic acid particles is 3 to 5: 2 to 4: 400 to 440; The preparation method of the KH-602 modified cerium zinc phenylphosphonate comprises the following steps: The zinc salt, cerium salt and phenylphosphonic acid are ultrasonically dispersed in deionized water, stirred for a certain period of time, and then refluxed, and then hydrothermally reacted, cooled to room temperature, washed, and dried to obtain zinc cerium phenylphosphonate; the obtained zinc cerium phenylphosphonate and KH-602 (N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane) are ultrasonically dispersed in ethanol water, and then stirred, cooled to room temperature, filtered, washed, and dried to obtain KH-602-modified zinc cerium phenylphosphonate; the molar ratio of the zinc salt, cerium salt and phenylphosphonic acid is: 0.1-0.3:0.7-0.9; 2; The preparation method of the SA-DOPO flame retardant comprises the following steps: Salicylaldehyde (SA) and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were ultrasonically dispersed in DMF, stirred under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and vacuum dried to obtain SA-DOPO; The molar ratio of SA to DOPO is 1:2.5-3.

5.

2. The method for preparing a garment fabric according to claim 1, wherein: In the preparation method of KH-602-modified zinc cerium phenylphosphonate, the zinc salt is at least one of zinc nitrate, zinc acetate, and zinc chloride, and the cerium salt is at least one of cerium nitrate, cerium acetate, and cerium chloride.

3. The method for preparing a garment fabric according to claim 1, wherein: In the preparation method of KH-602-modified cerium zinc phenylphosphonate, the stirring time is 20 to 40 minutes; the reflux reaction conditions are reflux reaction at 85 to 95° C. for 20 to 30 hours; the hydrothermal conditions are hydrothermal reaction at 100 to 140° C. for 16 to 24 hours; and the drying is drying at 80 to 100° C. for 10 to 14 hours.

4. The method for preparing a garment fabric according to claim 1, wherein: In the preparation method of KH-602-modified cerium zinc phenylphosphonate, the volume ratio of ethanol to water is 2:1; the mass ratio of cerium zinc phenylphosphonate to KH-602 is 10:0.5-0.9; and the stirring reaction is carried out at 40-60° C. for 2-4 hours.

5. The method for preparing a garment fabric according to claim 1, wherein: In the preparation method of the SA-DOPO flame retardant, the stirring reaction is carried out at 110-120° C. for 5-7 hours; and the vacuum drying is carried out at 70-90° C. for 12-20 hours.

6. Clothing fabric prepared according to the method for preparing clothing fabric according to any one of claims 1 to 5.

7. Use of the clothing fabric according to claim 6 in fireproof clothing.

Images