Garment fabric and preparation method and application thereof

By blending KH-602 modified zinc cerium phenylphosphonate and SA-DOPO flame retardant with polylactic acid particles, spinning and woven, garment fabrics with excellent flame retardant properties are solved, and the problem of flammability of polylactic acid fibers is achieved and safe application in the garment field is achieved.

CN119615468AActive Publication Date: 2025-03-14GUANGDONG BEISHUKANG NEW MATERIALS TECHNOLOGY CO LTD

Patent Information

Application Number
CN202411797499.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-09
Publication Date
2025-03-14
Estimated Expiration
2044-12-09

AI Technical Summary

Technical Problem

Polylactic fiber is flammable and produces a lot of heat and smoke when burning, limiting its wide application in the field of clothing.

Method used

By blending KH-602 modified zinc cerium phenylphosphonate and SA-DOPO flame retardant with polylactic acid particles, spinning and woven, garment fabrics with excellent flame retardant properties were produced.

Benefits of technology

This method significantly improves the flame retardant performance of the fabric, making it well used in the field of protective clothing, and maintains excellent flame retardant performance after multiple washes.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the technical field of fabrics, and particularly relates to a garment fabric and a preparation method and application thereof. 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, and then spinning to obtain polylactic acid fibers; and spinning and weaving the polylactic acid fibers to obtain the garment material. According to the invention, the KH-602 modified zinc and cerium phenylphosphonate and the SA-DOPO flame retardant are added, and interaction among the components is utilized to jointly promote the improvement of the flame retardant property of the fabric, so that the fabric is well applied to the field of protective clothing.
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Description

Technical Field

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

[0002] Polylactic acid fiber is a kind of fiber extracted from corn, wheat and other raw materials. This fiber does not use petroleum, has good biodegradability, biocompatibility and bioabsorbability, and has excellent mechanical properties of both synthetic fibers and natural fibers. It has received more and more attention and is a sustainable ecological fiber. However, polylactic acid fabrics are flammable, produce a lot of heat and smoke when burning, and are very likely to promote the spread of fire, causing serious harm to human production, life and even life, which to a certain extent limits the development and wide application of polylactic acid fabrics.

[0003] CN114921870A discloses a flame-retardant polylactic acid fabric and a preparation method thereof, wherein the fabric can be prepared by the following method: first, reacting terminal hydroxyl polydimethylsiloxane, dimethyl phosphate and hexachlorocyclotriphosphazene to prepare nitrogen-containing phosphorus silicon flame retardant; then, blending the nitrogen-containing phosphorus silicon flame retardant with polylactic acid particles, spinning to prepare polylactic acid fibers; finally, spinning and weaving the polylactic acid fibers to prepare flame-retardant polylactic acid fabric. The initial limiting oxygen index of the flame-retardant polylactic acid fabric prepared by the present invention reaches more than 35%, which belongs to the range of flame-retardant materials; after 10 times of water washing, the limiting oxygen index does not decrease significantly, and still reaches more than 32%. The flame-retardant polylactic acid fabric prepared by the method of the present invention has strong flame retardancy, the entire production process is simple, the price is low, and the production process has little environmental pollution.

[0004] CN113151922A discloses a flame retardant polylactic acid fiber elastic fabric and a preparation method thereof, and relates to the technical field of new materials. The invention first reacts phloroglucinol with an alkylating agent, and then continues to react with sodium lignin sulfonate under the action of potassium iodide to obtain modified lignin, then mixes the modified lignin with nano metal powder to obtain modified nano metal, then reacts bacterial cellulose with maleic anhydride to obtain modified bacterial cellulose, reacts the modified nano metal with epoxy soybean oil under the action of a tertiary amine catalyst, and then reacts with the modified bacterial cellulose to obtain a modified additive, and finally adds the modified additive and plasticizer to polyethylene, extrudes, melts and spins to obtain a polylactic acid fiber blank, and then hydrothermally carbonizes, spins and weaves the polylactic acid fiber blank to obtain a flame retardant polylactic acid fiber elastic fabric. The flame retardant polylactic acid fiber elastic fabric prepared by the invention has excellent conductivity and flame retardancy, and 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 and preparing the flame retardant components is high or the components are easily washed away, which results in a decrease in flame retardant properties after multiple washings. Summary of the invention

[0006] The technical problem to be solved by the present invention is to overcome the defects and shortcomings of the prior art and provide a clothing fabric and a preparation method and application thereof. The preparation method comprises the following steps: blending zinc cerium phenylphosphonate modified by KH-602, SA-DOPO flame retardant and polylactic acid particles at a certain temperature, and then spinning to obtain polylactic acid fibers; then spinning and weaving the polylactic acid fibers to obtain clothing fabrics. The present invention uses the interaction between the components to jointly promote the improvement of the flame retardant properties of the fabric by adding zinc cerium phenylphosphonate modified by KH-602 and SA-DOPO flame retardant, so that it can be well applied in the field of protective clothing.

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

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

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

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

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

[0012] The KH-602 modified zinc cerium phenylphosphonate, SA-DOPO flame retardant and polylactic acid particles are mixed at a certain temperature, and then spun to obtain polylactic acid fibers; the polylactic acid fibers are then 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 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, 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 for reaction, 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, the 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 for reaction 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 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 retardant 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 are also improved. SA-DOPO flame retardant is obtained by reacting salicylaldehyde with DOPO. SA-DOPO flame retardant is compounded with zinc cerium phenylphosphonate modified with KH-602 to jointly promote the improvement of 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, but the examples do not limit the present invention in any form. 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 are commercially available.

[0029] Example 1

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

[0031] 40g of KH-602 modified zinc cerium phenylphosphonate, 30g of SA-DOPO flame retardant and 4200g of polylactic acid particles were blended at 170°C, and then spun to obtain polylactic acid fibers; then the polylactic acid fibers were 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 is 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, stirred and reacted at 115 °C for 6 h under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and vacuum dried at 80 °C for 16 h to obtain SA-DOPO.

[0036] Example 2

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

[0038] 50g of KH-602 modified zinc cerium phenylphosphonate, 20g of SA-DOPO flame retardant and 4400g of polylactic acid particles were blended at 170°C, and then spun to obtain polylactic acid fibers; then the polylactic acid fibers were 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 zinc cerium phenylphosphonate; 10 g of zinc cerium phenylphosphonate and 0.9 g of KH-602 (N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane) were ultrasonically dispersed in 150 mL of ethanol water (the volume ratio of ethanol to water is 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 zinc cerium 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, stirred and reacted at 120 °C for 5 h under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and vacuum dried at 90 °C for 12 h to obtain SA-DOPO.

[0043] Example 3

[0044] A method for preparing a clothing fabric, the method 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; then the polylactic acid fibers were 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 is 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, stirred and reacted at 110°C for 7 h under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and vacuum dried 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 cerium phenylphosphonate modified with KH-602 is used to replace cerium zinc phenylphosphonate modified with KH-602.

[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 is 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 cerium zinc phenylphosphonate modified with KH-602.

[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 no SA-DOPO flame retardant is contained.

[0060] The flame retardant properties of Examples 1-3 and Comparative Examples 1-3 were tested, and 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 Color Fastness Tester Washing Method to carry out standard washing on the polylactic acid fabric.

[0062] Table 1:

[0063]

[0064] It can be seen from Table 1 that the clothing fabric prepared by the present invention has excellent flame retardant properties, and still has good flame retardant properties after 15 washes. That is, by comparing Example 1 with Comparative Examples 1-3, it can be seen that the addition of KH-602 modified zinc cerium phenylphosphonate and SA-DOPO flame retardant in the raw materials of the present invention can significantly improve the flame retardant properties 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 equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A method for preparing a clothing fabric, characterized in that: The preparation method comprises the following steps: The KH-602 modified zinc cerium phenylphosphonate, SA-DOPO flame retardant and polylactic acid particles are mixed at a certain temperature, and then spun to obtain polylactic acid fibers; the polylactic acid fibers are then spun and woven to obtain clothing fabrics.

2. The method for preparing a clothing fabric according to claim 1, characterized in that: The blending temperature is 165-175° C.; the mass ratio of the KH-602 modified cerium zinc phenylphosphonate, SA-DOPO flame retardant and polylactic acid particles is 3-5:2-4:400-440.

3. The method for preparing a clothing fabric according to claim 1, characterized in that: 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 for reaction, cooled to room temperature, filtered, washed, and dried to obtain KH-602-modified zinc cerium phenylphosphonate.

4. The method for preparing a clothing fabric according to claim 3, characterized in that: 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, the cerium salt, and phenylphosphonic acid is: 0.1-0.3:0.7-0.9; 2.

5. The method for preparing a clothing fabric according to claim 3, characterized in that: 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.

6. The method for preparing a clothing fabric according to claim 3, characterized in that: 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.

7. The method for preparing a clothing fabric according to claim 1, characterized in that: 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 for reaction under a nitrogen atmosphere, cooled to room temperature, distilled under reduced pressure, washed, and vacuum dried to obtain SA-DOPO.

8. The method for preparing a clothing fabric according to claim 7, characterized in that: 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.

9. Clothing fabric prepared according to the method for preparing clothing fabric according to any one of claims 1 to 8.

10. Use of the clothing fabric according to claim 9 in fireproof clothing.

Citation Information

Patent Citations

  • Flame-retardant polylactic acid fiber elastic fabric and preparation method thereof

    CN113151922A

  • Phosphorus-atom-containing oligomer composition, curable resin composition, substance resulting from curing same, and printed circuit board

    CN103249740A

  • Hydrophobic nano composite ocean anti-staining coating and preparation method thereof

    CN103265869A

  • Metal phenyl phosphonate flame-retardant material with controllable appearance, and preparation method and application thereof

    CN110643068A

  • Polylactic acid blending composition and preparation method thereof

    CN115960443A

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