Preparation method of efficient flame retardant and application of efficient flame retardant in textiles

By selecting suitable raw materials and preparation methods, a high-efficiency flame retardant was prepared, which solved the problems of poor stability and adhesion of flame retardant in the prior art, improved the flame retardant performance and wash resistance of textiles while maintaining the The softness of the hand feel.

CN119433991APending Publication Date: 2025-02-14TARIM UNIV +1
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Patent Information

Application Number
CN202411662824.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-20
Publication Date
2025-02-14

AI Technical Summary

Technical Problem

Existing textile flame retardants have problems such as poor stability, poor adhesion, and poor washing resistance, and poor hand feel of textiles.

Method used

By selecting suitable raw materials such as resin matrix, plastic matrix, phosphorus-containing compounds, metal compounds, polyols, film-forming agents, crosslinking agents and phytol hexaphosphate, and using specific ratios and preparation methods, a high-efficiency is prepared. Flame retardant and applied to textiles through rolling-baking-baking finishing process.

Benefits of technology

The flame retardant performance of textiles is improved, and the poor washing resistance caused by poor stability and adhesion of flame retardant is solved. At the same time, the softness and comfort of textiles are maintained, and the mechanical properties are good.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the technical field of flame-retardant finishing of textiles. The invention provides an efficient flame retardant. The efficient flame retardant is mainly prepared from the following raw materials in parts by weight: 15 to 20 parts of a resin matrix, 3 to 6 parts of a plastic matrix, 1 to 2.5 parts of a phosphorus-containing compound, 1 to 1.5 parts of a metal compound, 0.5 to 1.5 parts of polyol, 1 to 1.5 parts of a film-forming agent, 1 to 1.5 parts of a cross-linking agent and 1 to 1.5 parts of inositol hexaphosphate. Preferably, the resin matrix is selected from any one or a mixture of more of bisphenol A type epoxy resin, waterborne polyurethane resin, solvent type polyurethane resin, silane modified polyurethane resin and the like. The invention also provides a preparation method of the efficient flame retardant. The invention also provides application of the high-efficiency flame retardant in textiles. Through the selection of the raw materials and the reasonable ratio and the preparation method thereof, the efficient flame retardant is applied to the textile, the flame retardance of the textile is improved, and the problems that the flame retardant is poor in stability and adhesive force, poor in hand feeling of the textile and the like are solved.
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Description

Technical Field

[0001] The invention belongs to the technical field of flame retardant finishing of textiles, and particularly relates to a preparation method of a high-efficiency flame retardant and application thereof in textiles. Background Art

[0002] With the development of society and the improvement of people's living standards, higher requirements are placed on the safety and functionality of textiles. The flame retardant performance of textiles is one of the important aspects, especially in homes, public places and industrial production. Flame retardant textiles can effectively reduce the occurrence of fire accidents and protect people's lives and property.

[0003] At present, the flame retardants commonly used in textiles on the market mainly include halogen, phosphorus, nitrogen and inorganic flame retardants. Although these flame retardants have improved the flame retardancy of textiles to a certain extent, there are also some problems, such as poor stability of flame retardants, poor adhesion leading to poor washability, and poor feel of textiles.

[0004] For example, Chinese patent CN202110499471.1 discloses an inorganic-bio-based anti-light aging flame retardant and its application in textiles. The flame retardant of the invention includes gC prepared from urea. 3 N 4 anion suspension, a polyethyleneimine cation solution prepared with polyethyleneimine and deionized water, and a phytic acid anion solution prepared with phytic acid and deionized water. Mix the fluorescent powder, polyvinyl pyrrolidone and anhydrous ethanol, stir to obtain a coating solution; place the cotton fabric in the polyethyleneimine cation solution and gC 3 N 4 After alternately soaking in anionic solution, alternately soaking in polyethyleneimine cationic solution and phytic acid anionic solution, then evenly coating the coating solution and drying to obtain anti-light aging flame retardant cotton fabric. The flame retardant of the invention constructs an inorganic-bio-based hybrid self-assembled coating, effectively inhibits the afterburning of polyester-cotton fabric, improves the carbonization ability of cotton fabric, effectively absorbs ultraviolet rays through fluorescent powder, and enhances the anti-light aging performance of the fabric. However, on the one hand, the invention gC 3 N 4 The anionic suspension may precipitate or aggregate during long-term storage, which affects the use effect and has the problem of poor stability of the flame retardant. On the other hand, the polyethyleneimine in the invention is a cationic polymer, and its charge density may not be sufficient to react with gC 3 N 4 The anions and phytic acid anions form stable electrostatic adsorption, resulting in poor adhesion of flame retardants on textiles.

[0005] For example, Chinese patent CN202411226785.4 discloses a reactive phosphorus-nitrogen flame retardant and its preparation method and application. The preparation method of the reactive phosphorus-nitrogen flame retardant comprises the following steps: (1) reacting phosphorus oxychloride with pentaerythritol to generate pentaerythritol phosphoryl chloride; (2) reacting 1,3-butanediol and benzyl alcohol with pentaerythritol phosphoryl chloride to generate an intermediate product capped with 1,3-butanediol at one end and benzyl alcohol at the other end; (3) reacting the intermediate product with aminotrimethylenephosphonic acid to generate a reactive phosphorus-nitrogen flame retardant. The application of the reactive phosphorus-nitrogen flame retardant is to flame retardantly finish polyester / cotton blended fabrics. The obtained durable flame retardant polyester / cotton blended fabric has a limiting oxygen index higher than 31.5%, a damaged length lower than 8.1 cm, and a damaged length still lower than 14.3 cm after 55 washings, meeting the B1 standard, and having excellent flame retardant properties and water washability. However, since the phosphorus-nitrogen flame retardant generated by the reaction of the invention contains more rigid molecular structures, these structures may cause the treated textiles to become stiff and affect the hand feel.

[0006] Therefore, the prior art needs to be improved urgently. Summary of the invention

[0007] The present invention aims to provide a method for preparing a high-efficiency flame retardant and its application in textiles in view of the deficiencies of the prior art. The purpose of the present invention is to apply the prepared high-efficiency flame retardant to textiles through the selection of raw materials, reasonable proportions and preparation methods, thereby improving the flame retardant properties of textiles and solving the problems of poor stability of flame retardants, poor adhesion leading to poor washability, and poor feel of textiles.

[0008] To solve the above problems, the present invention provides the following technical solutions: A high-efficiency flame retardant is mainly prepared from the following raw materials in parts by weight: 15-20 parts of resin matrix, 3-6 parts of plastic matrix, 1-2.5 parts of phosphorus-containing compound, 1-1.5 parts of metal compound, 0.5-1.5 parts of polyol, 1-1.5 parts of film former, 1-1.5 parts of cross-linking agent, and 1-1.5 parts of phytate. Preferably, a high-efficiency flame retardant is mainly prepared from the following raw materials in parts by weight: 18-20 parts of resin matrix, 5-6 parts of plastic matrix, 1.5-2 parts of phosphorus-containing compound, 1-1.5 parts of metal compound, 1-1.5 parts of polyol, 1-1.5 parts of film former, 1-1.5 parts of cross-linking agent, and 1-1.5 parts of phytate. The most preferred embodiment is a high-efficiency flame retardant, which is mainly prepared from the following raw materials in parts by weight: 18 parts of resin matrix, 5 parts of plastic matrix, 2 parts of phosphorus-containing compound, 1 part of metal compound, 1 part of polyol, 1 part of film-forming agent, 1.5 parts of cross-linking agent, and 1.5 parts of inositol hexaphosphate.

[0009] In the high-efficiency flame retardant as described above, the resin matrix is ​​selected from any one of bisphenol A epoxy resin, waterborne polyurethane resin, solvent-based polyurethane resin, silane-modified polyurethane resin, waterborne acrylic resin, and solvent-based acrylic resin, or a mixture thereof. Preferably, the resin matrix is ​​selected from any one of waterborne polyurethane resin and waterborne acrylic resin, or a mixture thereof. Most preferably, the resin matrix is ​​selected from waterborne polyurethane resin. Under this condition, the waterborne polyurethane resin has good environmental protection and is easy to form a uniform and continuous film on the surface of textile fibers, thereby improving the adhesion and uniform distribution of the flame retardant. Moreover, the film has high transparency after forming, does not affect the original color and appearance of the textile, and is wear-resistant and scratch-resistant.

[0010] In the high-efficiency flame retardant as described above, the plastic matrix is ​​selected from any one of polyamide-imide, polyphenylene sulfide, polyether sulfone, polyamide, polyester or a mixture thereof. Most preferably, the plastic matrix is ​​selected from polyamide-imide. Under this condition, the glass transition temperature of polyamide-imide is high, ensuring the effectiveness and stability of the flame retardant in a high temperature environment, and its mechanical properties are good.

[0011] In the high-efficiency flame retardant as described above, the phosphorus-containing compound is selected from any one of ammonium polyphosphate, triphenyl phosphate, melamine cyanurate, and triethyl phosphate, or a mixture thereof. Most preferably, the phosphorus-containing compound is selected from melamine cyanurate. Under this condition, melamine cyanurate decomposes into non-combustible gas at high temperature to form an expanded carbon layer, which isolates oxygen and heat, thereby achieving a flame retardant effect. At the same time, it produces less smoke during the combustion process, thereby improving safety and visibility.

[0012] In the high-efficiency flame retardant as described above, the metal compound is selected from any one of zinc borate, aluminum hydroxide, and magnesium hydroxide, or a mixture thereof. Most preferably, the metal compound is selected from zinc borate. Under this condition, zinc borate decomposes at high temperature to generate insoluble zinc oxide and boric acid, which can form a protective layer to achieve a flame retardant effect, and can also absorb heat during the combustion process, reduce the temperature of the material, and slow down the combustion rate.

[0013] In the high-efficiency flame retardant as described above, the polyol is selected from any one of polyether polyol, polyester polyol, polycaprolactone polyol, and polycarbonate polyol, or a mixture thereof. Preferably, the polyol is selected from any one of polyester polyol and polycaprolactone polyol, or a mixture thereof. Most preferably, the polyol is selected from polycaprolactone diol, under which polycaprolactone diol has good thermal stability and low shrinkage at high temperatures, thereby maintaining the stability of the flame retardant.

[0014] As for the high-efficiency flame retardant as described above, the film-forming agent is selected from any one of polyacrylate, polyvinyl formal, polyvinyl butyral, sodium hydroxymethyl cellulose, hydroxypropyl methyl cellulose, and polyvinyl alcohol, or a mixture of several thereof. Preferably, the film-forming agent is selected from any one of sodium hydroxymethyl cellulose and hydroxypropyl methyl cellulose, or a mixture of the two. Under this condition, sodium hydroxymethyl cellulose and hydroxypropyl methyl cellulose have good film-forming effect, will not affect the original color and appearance of textiles, have good flexibility, and have good dispersibility with other raw material components of flame retardants, thereby improving the treatment effect. Most preferably, the film-forming agent is selected from sodium hydroxymethyl cellulose.

[0015] As for the high-efficiency flame retardant as described above, the crosslinking agent is selected from any one of 3-glycidyloxypropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, and N,N-bis(3-trimethoxysilylpropyl)amine, or a mixture thereof. Preferably, the crosslinking agent is selected from any one of 3-aminopropyltrimethoxysilane and 3-aminopropyltriethoxysilane. Under this condition, 3-aminopropyltrimethoxysilane and 3-aminopropyltriethoxysilane have high reactivity, which can improve the bonding force between the flame retardant and the textile fiber, and can be compounded with the raw material components of other flame retardants such as resin matrix, plastic matrix, etc. through amino groups to improve the stability of the flame retardant. Most preferably, the crosslinking agent is selected from 3-aminopropyltrimethoxysilane.

[0016] Based on the same inventive concept, the present invention provides a method for preparing the above-mentioned high-efficiency flame retardant, comprising the following steps: (1) According to the set raw material ratio, the resin matrix and the plastic matrix are placed in a reactor, mixed evenly, and stirred for 20 to 40 minutes to obtain a mixture 1; (2) Adding a phosphorus-containing compound and a metal compound in a set ratio to the mixture 1, mixing them evenly, and stirring for 30 to 60 minutes to obtain a mixture 2; (3) Add a set ratio of polyol, film-forming agent, cross-linking agent and inositol hexaphosphate to mixture 2, mix well, and stir for 60 to 120 minutes to obtain a high-efficiency flame retardant.

[0017] In the present invention, the resin matrix and the plastic matrix are mixed uniformly by mechanical stirring to ensure that the two matrix materials are fully contacted and dispersed. During the stirring process, the water-based polyurethane resin and water-based acrylic resin as the resin matrix and the polyamide-imide as the plastic matrix are preliminarily chemically cross-linked to form a network structure, which helps to provide adhesion and dispersibility of other subsequent raw materials; melamine cyanurate decomposes at high temperature to generate non-combustible gas (such as ammonia and nitrogen), forming an expanded carbon layer to isolate oxygen and heat; zinc borate decomposes at high temperature to generate insoluble zinc oxide and boric acid, these products can form a protective layer, absorb heat, and reduce the temperature of the material; melamine cyanurate and zinc borate work synergistically to form multiple flame retardant mechanisms by generating non-combustible gas and a protective layer, which significantly improves Flame retardant effect; the hydroxyl groups in polyester polyols can be chemically cross-linked with waterborne polyurethane resins or waterborne resins and polyamide-imide to improve the mechanical properties and flexibility of the flame retardant coating; the hydroxyl groups in sodium hydroxymethyl cellulose or hydroxypropyl methyl cellulose can be physically adsorbed or chemically bonded with the functional groups in waterborne polyurethane resins or waterborne acrylic resins, polyamide-imide, and polyester polyols to increase the viscosity of the flame retardant solution, thereby ensuring the uniformity of film formation; inositol hexaphosphate can chelate with melamine cyanurate, zinc borate, metal ions and functional groups in waterborne polyurethane resins or waterborne acrylic resins, polyamide-imide, and polyester polyols to form a stable flame retardant complex, thereby improving the stability and antioxidant properties of the prepared flame retardant. The synergistic effect of the above various raw materials and their proportions solves the problems of poor stability of flame retardants in the prior art, poor adhesion leading to poor washability, and poor feel of textiles.

[0018] Based on the same inventive concept, the present invention provides an application of the high-efficiency flame retardant as described above or the high-efficiency flame retardant prepared by the preparation method as described above in textiles. Preferably, the textile is a cotton textile. Preferably, the application method comprises the following steps: applying the high-efficiency flame retardant to the cotton textile through a finishing process of rolling-baking-curing to obtain a cotton textile with flame retardant properties. Specifically, the application method comprises the following steps: S1. Pretreatment: Clean the cotton textile thoroughly to remove grease, impurities and slurry on the surface to ensure that the surface of the textile is clean, and immerse the cleaned cotton textile in the above-mentioned high-efficiency flame retardant solution to ensure that the cotton textile fully absorbs moisture; S2. Pad dyeing: The impregnated cotton textile is passed through a padder to remove excess flame retardant solution, and the liquid carrying rate of the cotton textile is controlled at 60%-80% to ensure that the flame retardant is evenly distributed on the cotton textile; S3, drying: put the cotton textile after pad dyeing into the drying machine, control the temperature at 80-100℃, and dry for 5-10min. Under this condition, it is to ensure that the cotton textile is completely dried; S4, baking: put the dried cotton textile into a baking machine, control the temperature at 150-180℃, and the baking time is 2-5min; under this condition, if the baking temperature is too high and the baking time is too long, for example, the baking temperature exceeds 180℃ and the drying time is longer than 5min, high temperature or long drying time will damage the cotton fiber. If the baking temperature is lower than 150℃ and the drying time is less than 2min, the baking effect will be affected. Control the temperature at 150-180℃ and the drying time at 2-5min. In this process, the flame retardant and the cotton fiber can undergo a cross-linking reaction to form a stable flame retardant layer; S5, post-finishing: The baked cotton textile in step S4 is subjected to shaping treatment. This step ensures the dimensional stability and hand feel of the cotton textile, thereby obtaining a cotton textile with flame retardant properties.

[0019] Compared with the existing technology, the effects and advantages of the present invention are: 1. The present invention provides a high-efficiency flame retardant, which is mainly prepared from the following raw materials in parts by weight: 15 to 20 parts of a resin matrix, 3 to 6 parts of a plastic matrix, 1 to 2.5 parts of a phosphorus-containing compound, 1 to 1.5 parts of a metal compound, 0.5 to 1.5 parts of a polyol, 1 to 1.5 parts of a film-forming agent, 1 to 1.5 parts of a cross-linking agent, and 1 to 1.5 parts of inositol hexaphosphate. The high-efficiency flame retardant has a good flame retardant effect, ensures the stability and durability of the flame retardant, maintains the softness and comfort of the textiles, and has good mechanical properties, and is suitable for the application of high-performance textile flame retardants.

[0020] 2. The preparation method of a high-efficiency flame retardant provided by the present invention is simple. By adding raw materials step by step and stirring them fully, it is ensured that the raw materials are evenly dispersed and fully mixed in the flame retardant system, thereby improving the stability of the final product.

[0021] 3. The application of a high-efficiency flame retardant in textiles provided by the present invention is particularly suitable for cotton textiles. Through a rolling-drying-baking finishing process, the high-efficiency flame retardant is applied to cotton textiles to obtain cotton textiles with flame retardant properties. The pretreatment is thorough so that the flame retardant is evenly distributed, and efficient drying and moderate baking are performed to avoid damage to the cotton fibers. The post-finishing improves the performance. The steps are simple, easy to control, and suitable for large-scale industrial production. DETAILED DESCRIPTION

[0022] The following will combine the contents in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] Unless otherwise defined, all technical and scientific terms used in this specification have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used in this specification includes any and all combinations of one or more of the related listed items.

[0024] Unless otherwise specified, the experimental methods used in the following examples are conventional methods.

[0025] Unless otherwise specified, the materials and reagents used in the following examples can be obtained from commercial sources. Melamine cyanurate was purchased from Guangzhou Yinyuan New Material Technology Co., Ltd.; Embodiment 1: The present embodiment provides a high-efficiency flame retardant, which is mainly prepared from the following raw materials in parts by weight: 18 parts of resin matrix, 5 parts of plastic matrix, 2 parts of phosphorus-containing compound, 1 part of metal compound, 1 part of polyol, 1 part of film former, 1.5 parts of cross-linking agent, and 1.5 parts of inositol hexaphosphate. In this embodiment, the resin matrix is ​​water-based polyurethane resin; the plastic matrix is ​​polyamide-imide; the phosphorus-containing compound is melamine cyanurate, CAS number: 37640-57-6, molecular weight: 255.2; the metal compound is zinc borate; the polyol is polycaprolactone diol; the film former is sodium hydroxymethyl cellulose; and the cross-linking agent is 3-aminopropyltrimethoxysilane.

[0026] The present embodiment provides a high-efficiency flame retardant, which is prepared by the following preparation method, which specifically comprises the following steps: (1) According to the set raw material ratio, the resin matrix and the plastic matrix are placed in a reactor, mixed evenly, stirred at a speed of 200 rpm, and stirred for 30 minutes to obtain a mixture 1; (2) Adding a phosphorus-containing compound and a metal compound in a set ratio to the mixture 1, mixing them evenly, stirring at a speed of 300 rpm for 40 minutes, and obtaining a mixture 2; (3) Add a set ratio of polyol, film-forming agent, cross-linking agent and inositol hexaphosphate to mixture 2, mix well, stir at a speed of 300 rpm, and stir for 60 minutes to obtain a high-efficiency flame retardant.

[0027] Embodiment 2: The present embodiment provides a high-efficiency flame retardant, which is mainly prepared from the following raw materials in parts by weight: 20 parts of resin matrix, 6 parts of plastic matrix, 1.5 parts of phosphorus-containing compound, 1.5 parts of metal compound, 1 part of polyol, 1.5 parts of film former, 1 part of cross-linking agent, and 1.5 parts of inositol hexaphosphate. In this embodiment, the resin matrix is ​​waterborne polyurethane resin; the plastic matrix is ​​polyamide-imide; the phosphorus-containing compound is melamine cyanurate, CAS number: 37640-57-6, molecular weight: 255.2; the metal compound is zinc borate; the polyol is polycaprolactone diol; the film former is a mixture of sodium hydroxymethyl cellulose and hydroxypropyl methyl cellulose, and the mass ratio of sodium hydroxymethyl cellulose to hydroxypropyl methyl cellulose is 1:1; the cross-linking agent is 3-aminopropyl trimethoxy silane.

[0028] The present embodiment provides a high-efficiency flame retardant, which is prepared by the following preparation method, which specifically comprises the following steps: (1) According to the set raw material ratio, the resin matrix and the plastic matrix are placed in a reactor, mixed evenly, stirred at a speed of 200 rpm, and stirred for 20 minutes to obtain a mixture 1; (2) Adding a phosphorus-containing compound and a metal compound in a set ratio to the mixture 1, mixing them evenly, stirring at a speed of 300 rpm for 60 minutes, and obtaining a mixture 2; (3) Add a set ratio of polyol, film-forming agent, cross-linking agent and inositol hexaphosphate to mixture 2, mix well, stir at a speed of 300 rpm, and stir for 80 minutes to obtain a high-efficiency flame retardant.

[0029] Embodiment 3: The present embodiment provides a high-efficiency flame retardant, which is mainly prepared from the following raw materials in parts by weight: 18 parts of resin matrix, 5 parts of plastic matrix, 2 parts of phosphorus-containing compound, 1 part of metal compound, 1 part of polyol, 1 part of film former, 1.5 parts of cross-linking agent, and 1.5 parts of inositol hexaphosphate. In this embodiment, the resin matrix is ​​waterborne polyurethane resin; the plastic matrix is ​​polyamide-imide; the phosphorus-containing compound is melamine cyanurate, CAS number: 37640-57-6, molecular weight: 255.2; the metal compound is zinc borate; the polyol is polycaprolactone diol; the film former is sodium hydroxymethyl cellulose; and the cross-linking agent is 3-aminopropyl triethoxysilane.

[0030] The present embodiment provides a high-efficiency flame retardant, which is prepared by the following preparation method, which specifically comprises the following steps: (1) According to the set raw material ratio, the resin matrix and the plastic matrix are placed in a reactor, mixed evenly, stirred at a speed of 150 rpm for 30 minutes, and a mixture 1 is obtained; (2) Adding a phosphorus-containing compound and a metal compound in a set ratio to the mixture 1, mixing them evenly, stirring at a speed of 300 rpm for 60 minutes, and obtaining a mixture 2; (3) Add a set ratio of polyol, film-forming agent, cross-linking agent and inositol hexaphosphate to mixture 2, mix well, stir at a speed of 300 rpm, and stir for 120 minutes to obtain a high-efficiency flame retardant.

[0031] Embodiment 4: The present embodiment provides a high-efficiency flame retardant, which is mainly prepared from the following raw materials in parts by weight: 15 parts of resin matrix, 6 parts of plastic matrix, 2.5 parts of phosphorus-containing compound, 1.5 parts of metal compound, 1.5 parts of polyol, 1 part of film former, 1.5 parts of cross-linking agent, and 1.5 parts of inositol hexaphosphate. In this embodiment, the resin matrix is ​​waterborne polyurethane resin; the plastic matrix is ​​polyamide-imide; the phosphorus-containing compound is melamine cyanurate, CAS number: 37640-57-6, molecular weight: 255.2; the metal compound is zinc borate; the polyol is polycaprolactone diol; the film former is sodium hydroxymethyl cellulose; and the cross-linking agent is 3-aminopropyltrimethoxysilane.

[0032] The present embodiment provides a high-efficiency flame retardant, which is prepared by the following preparation method, which specifically comprises the following steps: (1) According to the set raw material ratio, the resin matrix and the plastic matrix are placed in a reactor, mixed evenly, stirred at a speed of 200 rpm, and stirred for 30 minutes to obtain a mixture 1; (2) Adding a phosphorus-containing compound and a metal compound in a set ratio to the mixture 1, mixing them evenly, stirring at a speed of 200 rpm for 40 minutes, and obtaining a mixture 2; (3) Add a set ratio of polyol, film-forming agent, cross-linking agent and inositol hexaphosphate to mixture 2, mix well, stir at a speed of 300 rpm, and stir for 100 minutes to obtain a high-efficiency flame retardant.

[0033] Embodiment 5: The present embodiment provides a high-efficiency flame retardant, which is mainly prepared from the following raw materials in parts by weight: 18 parts of resin matrix, 5 parts of plastic matrix, 2 parts of phosphorus-containing compound, 1 part of metal compound, 1 part of polyol, 1 part of film former, 1.5 parts of cross-linking agent, and 1.5 parts of inositol hexaphosphate. In this embodiment, the resin matrix is ​​water-based acrylic resin; the plastic matrix is ​​polyamide-imide; the phosphorus-containing compound is melamine cyanurate, CAS number: 37640-57-6, molecular weight: 255.2; the metal compound is zinc borate; the polyol is polycaprolactone diol; the film former is sodium hydroxymethyl cellulose; and the cross-linking agent is 3-aminopropyl triethoxysilane.

[0034] The present embodiment provides a high-efficiency flame retardant, which is prepared by the following preparation method, which specifically comprises the following steps: (1) According to the set raw material ratio, the resin matrix and the plastic matrix are placed in a reactor, mixed evenly, stirred at a speed of 200 rpm, and stirred for 30 minutes to obtain a mixture 1; (2) Adding a phosphorus-containing compound and a metal compound in a set ratio to the mixture 1, mixing them evenly, stirring at a speed of 300 rpm for 40 minutes, and obtaining a mixture 2; (3) Add a set ratio of polyol, film-forming agent, cross-linking agent and inositol hexaphosphate to mixture 2, mix well, stir at a speed of 300 rpm, and stir for 60 minutes to obtain a high-efficiency flame retardant.

[0035] Comparative Example 1: This comparative example is basically the same as Example 1, except that polycaprolactone diol is not added in step (3).

[0036] Comparative Example 2: This comparative example is substantially the same as Example 1, except that 3-aminopropyltrimethoxysilane is not added in step (3).

[0037] Comparative Example 3: A commercially available phosphorus flame retardant with a density of 1.2 g / cm 3 , flash point>100℃, insoluble in water, soluble in organic solvents.

[0038] Application examples: The flame retardant described in Examples 1 to 5 and Comparative Examples 1 to 3 is applied to textiles. The textile selected in this application example is a cotton textile. This application example uses 100% cotton fabric, with a gram weight of 200 g / m², a warp and weft density of 80×80, a yarn count of 21×21, a twill fabric, a bleached white color, and a sample size of 30cm×30cm. The application method includes the following steps: applying the high-efficiency flame retardant to the cotton textile through a rolling-baking-baking finishing process to obtain a cotton textile with flame retardant properties. Specifically, the application method includes the following steps: S1. Pretreatment: Clean the cotton textile thoroughly to remove grease, impurities and slurry on the surface to ensure that the surface of the textile is clean, and immerse the cleaned cotton textile in the above-mentioned high-efficiency flame retardant solution to ensure that the cotton textile fully absorbs moisture; S2. Pad dyeing: The impregnated cotton textile is passed through a padder to remove excess flame retardant solution, and the liquid carrying rate of the cotton textile is controlled at 70% to ensure that the flame retardant is evenly distributed on the cotton textile; S3, drying: putting the cotton textile after pad dyeing into a drying machine, controlling the temperature at 90°C and the drying time for 10 minutes, under this condition, the cotton textile is ensured to be completely dried; S4. Baking: Put the dried cotton textile into a baking machine, control the temperature at 160°C, and bake for 5 minutes; the surface of the dried sample is flat and has no cracks; S5, post-finishing: The baked cotton textile in step S4 is subjected to shaping treatment. This step ensures the dimensional stability and hand feel of the cotton textile, thereby obtaining a cotton textile with flame retardant properties.

[0039] According to relevant standards, the flame retardant test performance of the cotton textile obtained above, the flame retardant performance after washing, the tensile property, the tearing property and the abrasion resistance of the fabric sample were evaluated. The results are shown in Table 1.

[0040] Table 1 Performance evaluation results of Examples 1 to 5 and Comparative Examples 1 to 3

[0041] It can be seen from Table 1 that the flame retardant treated cotton fabrics prepared in Examples 1 to 5 of the present invention have better performance than those in Comparative Examples 1 to 3, and in particular, it can be seen from the flame retardant performance after washing that Comparative Examples 1 and 2 are significantly lower than the present invention, indicating that the flame retardant stability of the present invention is better, whether it is flame retardant performance, tensile performance, tear performance, abrasion resistance, or environmental protection, in terms of comprehensive performance, it is shown that the flame retardant product prepared by the present invention has excellent performance, outstanding flame retardant performance, good adhesion, good stability, and good mechanical properties.

[0042] It should be pointed out that the specific implementation methods are only representative examples of the present invention. Obviously, the technical solution of the present invention is not limited to the above-mentioned embodiments, and there are many variations. Those skilled in the art who can obtain the invention clearly disclosed in the present invention or without objection based on the written description of the document should be considered as the scope of protection of this patent.

Claims

1. A high efficiency flame retardant, characterized in that: It is mainly prepared from the following raw materials in parts by weight: 15-20 parts of resin matrix, 3-6 parts of plastic matrix, 1-2.5 parts of phosphorus-containing compound, 1-1.5 parts of metal compound, 0.5-1.5 parts of polyol, 1-1.5 parts of film-forming agent, 1-1.5 parts of cross-linking agent and 1-1.5 parts of inositol hexaphosphate.

2. The high-efficiency flame retardant according to claim 1, characterized in that: The resin matrix is ​​selected from any one of bisphenol A epoxy resin, waterborne polyurethane resin, solvent-based polyurethane resin, silane-modified polyurethane resin, waterborne acrylic resin, and solvent-based acrylic resin, or a mixture of several of them.

3. The high-efficiency flame retardant according to claim 1, characterized in that: The plastic matrix is ​​selected from any one of polyamide-imide, polyphenylene sulfide, polyethersulfone, polyamide and polyester or a mixture of several thereof.

4. The high-efficiency flame retardant according to claim 1, characterized in that: The phosphorus-containing compound is selected from any one of ammonium polyphosphate, triphenyl phosphate, melamine cyanurate, and triethyl phosphate, or a mixture of several of them.

5. The high-efficiency flame retardant according to claim 1, characterized in that: The metal compound is selected from any one of zinc borate, aluminum hydroxide and magnesium hydroxide or a mixture of several thereof.

6. The high-efficiency flame retardant according to claim 1, characterized in that: The polyol is selected from any one of polyether polyol, polyester polyol, polycaprolactone polyol and polycarbonate polyol or a mixture of several thereof.

7. The high-efficiency flame retardant according to claim 1, characterized in that: The film-forming agent is selected from any one of polyacrylate, polyvinyl formal, polyvinyl butyral, sodium hydroxymethyl cellulose, hydroxypropyl methyl cellulose, and polyvinyl alcohol, or a mixture of several of them.

8. The high-efficiency flame retardant according to claim 1, characterized in that: The crosslinking agent is selected from any one of 3-glycidyloxypropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, and N,N-bis(3-trimethoxysilylpropyl)amine or a mixture of several thereof.

9. A method for preparing a high-efficiency flame retardant according to any one of claims 1 to 7, characterized in that: The following steps are involved: (1) According to the set raw material ratio, the resin matrix and the plastic matrix are placed in a reactor, mixed evenly, and stirred for 20 to 40 minutes to obtain a mixture 1; (2) Adding a phosphorus-containing compound and a metal compound in a set ratio to the mixture 1, mixing them evenly, and stirring for 30 to 60 minutes to obtain a mixture 2; (3) Add a set ratio of polyol, film-forming agent, cross-linking agent and inositol hexaphosphate to mixture 2, mix well, and stir for 60 to 120 minutes to obtain a high-efficiency flame retardant.

10. Use of the high-efficiency flame retardant according to any one of claims 1 to 7 or the high-efficiency flame retardant prepared by the preparation method according to claim 8 in textiles.

Citation Information

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