Preparation process of halogen-free flame-retardant polyester cotton fabric

Abstract

The invention relates to the field of textile materials, in particular to a preparation process of a halogen-free flame-retardant polyester-cotton fabric, which is used for solving the problems that the existing polyester-cotton fabric is poor in flame-retardant property, and the flame-retardant fabric is easily harmful to the environment and human health due to the fact that the flame-retardant fabric is mostly treated by adopting a halogen-containing compound. The halogen-free flame retardant is adopted, the problem that a traditional halogen-containing flame retardant generates toxic gas during combustion is solved, the environment-friendly requirement is met, the flame-retardant polyester fibers are blended, so that the fabric has excellent flame retardance and is suitable for the fields of electric power protective clothing and firefighter uniform, the preparation process is relatively simple, industrial production is easy, and the fabric is worthy of popularization and application. And the production cost is reduced.

Description

Technical Field

[0001] The invention relates to the field of textile materials, and in particular to a preparation process of a halogen-free flame-retardant polyester-cotton fabric. Background Art

[0002] Polyester-cotton refers to the general term for blended fabrics of polyester and cotton. Textiles woven with polyester and cotton blended yarns are commonly known as "Dacron". It not only maintains the high strength and good elastic recovery characteristics of polyester fibers, but also has the characteristics of strong hygroscopicity of cotton fibers. It is easy to dye, does not require ironing and dries quickly after washing. It is a common material for making clothes and is widely used, especially in clothing. The market is huge. With the increasing demand for protective clothing in the fields of fire protection, electricity, and the military, higher requirements are placed on the flame retardant properties of textile fabrics. Traditional polyester-cotton fabrics are easy to burn when encountering a fire source, causing safety hazards. Currently, most flame-retardant fabrics on the market are treated with halogen-containing compounds, but these compounds produce toxic gases when burned, causing harm to the environment and human health. Therefore, it is of great practical significance to develop a halogen-free flame-retardant polyester-cotton fabric that is both environmentally friendly and efficient. Summary of the invention

[0003] In order to overcome the above technical problems, the purpose of the present invention is to provide a preparation process of halogen-free flame-retardant polyester-cotton fabric, which solves the problem that the existing polyester-cotton fabric has poor flame retardant performance and the flame retardant fabric is mostly treated with halogen-containing compounds, which is easy to cause harm to the environment and human health.

[0004] The purpose of the present invention can be achieved through the following technical solutions: A preparation process of a halogen-free flame-retardant polyester-cotton fabric comprises the following steps: Step 1: Weigh 76-82 parts of polyester resin and 4.8-12.2 parts of composite flame retardant according to weight; the model of the polyester resin is JT-B1; Step 2: Evenly mix the polyester resin and the composite flame retardant, and then melt extrude the mixture through a twin-screw extruder, cool and pelletize the mixture, and then melt spin the mixture to obtain a flame-retardant polyester fiber; Step 3: blending the flame retardant polyester fiber and the cotton fiber in a mass ratio of 65:35 to obtain polyester-cotton yarn; Step 4: Weaving the polyester-cotton yarn into polyester-cotton fabric to obtain halogen-free flame-retardant polyester-cotton fabric.

[0005] As a further solution of the present invention: the composite flame retardant is prepared by the following steps: Step s1: adding melamine, terephthalaldehyde, anhydrous sodium acetate and anhydrous ethanol into a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a reflux condenser, introducing nitrogen protection, stirring the reaction at a temperature of 20-25° C. and a stirring rate of 300-400 r / min for 15-25 min, then heating to reflux and continuing to stir the reaction for 4-5 h, after the reaction is completed, cooling the reaction product to room temperature, and then rotary evaporating to remove the solvent to obtain intermediate 1; Step s2: Add intermediate 1, 3-aminopropyltriethoxysilane, anhydrous sodium acetate and anhydrous ethanol into a three-necked flask equipped with a stirrer, a thermometer and an air duct, introduce nitrogen protection, stir and react for 20-30 minutes at a temperature of 20-25° C. and a stirring rate of 300-400 r / min, then heat to 80-85° C. and continue stirring and reacting for 6-7 hours. After the reaction is completed, cool the reaction product to room temperature, and then remove the solvent by rotary evaporation to obtain intermediate 2; Step s3: Add intermediate 2, DOPO and anhydrous ethanol to a three-necked flask equipped with a stirrer, a thermometer and an air duct, introduce nitrogen protection, stir and react for 15-20 minutes at a temperature of 80-85°C and a stirring rate of 300-400r / min, then heat to 100-110°C and continue stirring and reacting for 10-12 hours. After the reaction is completed, cool the reaction product to room temperature, then rotary evaporate to remove the solvent, then add it to ice water, then let it stand to precipitate, then vacuum filter, place the filter cake in a vacuum drying oven, and dry it at a temperature of 60-65°C for 2-3 hours to obtain an organic multi-effect flame retardant; Step s4: adding anhydrous magnesium sulfate and deionized water to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, stirring and reacting for 15-20 minutes at a temperature of 20-25°C and a stirring rate of 300-400r / min, then adding activated carbon and sodium dodecylbenzenesulfonate and continuing to stir and react for 15-20 minutes, then adding ammonia water dropwise while stirring, controlling the dropping rate to 1-2 drops / s, and continuing to stir and react for 10-15 hours at a temperature of 45-55°C after the dropwise addition is completed. After the reaction is completed, the reaction product is cooled to room temperature, then centrifuged, and the precipitate is washed with distilled water 2-3 times, then placed in a vacuum drying oven, and dried at a temperature of 55-60°C for 2-3 hours to obtain an inorganic multi-effect flame retardant; Step s5: Add an organic multi-effect flame retardant, anhydrous ethanol and deionized water to a three-necked flask equipped with an agitator, a thermometer and an air duct, introduce nitrogen protection, stir and react for 15-20 minutes at a temperature of 20-25°C and a stirring rate of 300-400r / min, then adjust the pH to 2-3 with anhydrous acetic acid, and continue to stir and react for 5-10 minutes, then add an inorganic multi-effect flame retardant and continue to stir and react for 5-6 hours under the condition of raising the temperature to 75-80°C. After the reaction is completed, the reaction product is cooled to room temperature and then centrifuged. The precipitate is washed with distilled water 2-3 times, and then placed in a vacuum drying oven and dried at a temperature of 55-60°C for 2-3 hours to obtain a composite flame retardant.

[0006] As a further solution of the present invention: the usage ratio of melamine, terephthalaldehyde, anhydrous sodium acetate and anhydrous ethanol in step s1 is 10 mmol: 30 mmol: 0.05-0.15 g: 50-55 mL.

[0007] As a further solution of the present invention: the usage ratio of the intermediate 1, 3-aminopropyltriethoxysilane, anhydrous sodium acetate and anhydrous ethanol in step s2 is 10 mmol: 30 mmol: 0.08-0.16 g: 60-70 mL.

[0008] As a further solution of the present invention: the usage ratio of the intermediate 2, DOPO and anhydrous ethanol in step s3 is 10 mmol:60 mmol:100-120 mL.

[0009] As a further solution of the present invention: the usage ratio of the anhydrous magnesium sulfate, deionized water, activated carbon, sodium dodecylbenzene sulfonate and ammonia water in step s4 is 10-15g:45-50mL:3g:0.2-0.6g:15-25mL.

[0010] As a further solution of the present invention: the mass fraction of the ammonia water in step s4 is 20-25%.

[0011] As a further solution of the present invention: the usage ratio of the organic multi-effect flame retardant, anhydrous ethanol, deionized water and inorganic multi-effect flame retardant in step s5 is 2-10g:40-45mL:5-10mL:5g.

[0012] Beneficial effects of the present invention: The invention discloses a preparation process of a halogen-free flame-retardant polyester-cotton fabric. The process comprises the following steps: uniformly mixing a polyester resin and a composite flame retardant, then melt-extruding, cooling, pelletizing, and then melt-spinning to obtain a flame-retardant polyester fiber. The flame-retardant polyester fiber and cotton fiber are blended to obtain a polyester-cotton yarn. The polyester-cotton yarn is woven into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric. The invention adopts a halogen-free flame retardant to avoid the problem that traditional halogen-containing flame retardants generate toxic gases during combustion, thus meeting environmental protection requirements. By preparing the flame-retardant polyester fiber for blending, the fabric has excellent flame-retardant properties and is suitable for the fields of power protective clothing and firefighting clothing. The preparation process of the invention is relatively simple, easy to industrialize, and reduces production costs.

[0013] In the process of preparing halogen-free flame-retardant polyester-cotton fabric, a composite flame retardant is first prepared. First, melamine and terephthalaldehyde are reacted. The amino group on melamine reacts with an aldehyde group on terephthalaldehyde to form a C=N bond, and an aldehyde group is introduced to obtain intermediate 1. Then, intermediate 1 reacts with 3-aminopropyltriethoxysilane. The aldehyde group on intermediate 1 reacts with the amino group on 3-aminopropyltriethoxysilane to form a C=N bond, and a large number of siloxane groups are introduced to obtain intermediate 2. Then, intermediate 2. DOPO reaction: the C=N bond on the intermediate 2 reacts with the PH bond on the DOPO to introduce organic phosphorus to obtain an organic multi-effect flame retardant. Then, anhydrous magnesium sulfate, ammonia water and activated carbon are reacted to form magnesium hydroxide on the surface of the activated carbon to form a composite structure of magnesium hydroxide wrapped in activated carbon to obtain an inorganic multi-effect flame retardant. Then, the inorganic multi-effect flame retardant is treated with the organic multi-effect flame retardant. The siloxane groups on the organic multi-effect flame retardant are hydrolyzed to form silanols, which can be grafted to the particle surface of the inorganic multi-effect flame retardant after dehydration condensation. A composite flame retardant is obtained; the activated carbon in the composite flame retardant has an extremely high surface area and a uniform pore size distribution, which enables it to effectively adsorb organic matter, impurities and combustible gases, and also forms a carbon layer on the surface of the material, which can block the direct contact between the substrate and the air, thereby achieving a flame retardant effect; the magnesium hydroxide wrapped on the surface of the activated carbon can absorb a large amount of heat during thermal decomposition, and at the same time generate a large amount of water vapor and high-temperature resistant metal oxides to play a flame retardant role; the organic multi-effect flame retardant grafted on the surface of the magnesium hydroxide can effectively improve the dispersibility of the composite flame retardant, so that it can be evenly dispersed in the flame-retardant polyester fiber, thereby achieving an excellent flame retardant effect; and the organic multi-effect flame retardant contains a large amount of organic phosphorus and organic nitrogen in its molecular structure, and under the synergistic effect of the two, the concentration of combustible gases can be reduced, and the formation of a carbon layer can be promoted, thereby effectively preventing the spread of flames and achieving a flame retardant effect; therefore, under the synergistic effect of the organic multi-effect flame retardant and the inorganic multi-effect flame retardant, the composite flame retardant is given a high flame retardant effect, so that the prepared polyester-cotton fabric has excellent flame retardant properties. DETAILED DESCRIPTION

[0014] The following will be combined with 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.

[0015] Embodiment 1: This embodiment is a preparation process of a halogen-free flame-retardant polyester-cotton fabric, comprising the following steps: Step A1: 10 mmol melamine, 30 mmol terephthalaldehyde, 0.05 g anhydrous sodium acetate and 50 mL anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen was introduced for protection. The mixture was stirred at 20° C. and a stirring rate of 300 r / min for 15 min, and then the temperature was raised to reflux and the stirring reaction was continued for 4 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 1; Step A2: 10 mmol of intermediate 1, 30 mmol of 3-aminopropyltriethoxysilane, 0.08 g of anhydrous sodium acetate and 60 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 20° C. and a stirring rate of 300 r / min for 20 min, and then the temperature was raised to 80° C. and the stirring reaction was continued for 6 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 2; Step A3: 10 mmol of intermediate 2, 60 mmol of DOPO and 100 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred at 80° C. and a stirring rate of 300 r / min for 15 min, and then the mixture was heated to 100° C. and the stirring reaction was continued for 10 h. After the reaction, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The product was then added to ice water, and then allowed to stand to precipitate. The product was then vacuum filtered, and the filter cake was placed in a vacuum drying oven and dried at 60° C. for 2 h to obtain an organic multi-effect flame retardant. Step A4: 10 g of anhydrous magnesium sulfate and 45 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and the mixture was stirred for 15 min at a temperature of 20° C. and a stirring rate of 300 r / min. Then, 3 g of activated carbon and 0.2 g of sodium dodecylbenzene sulfonate were added and the stirring reaction was continued for 15 min. Then, 15 mL of 20% ammonia water by mass was added dropwise while stirring, and the dropping rate was controlled to be 1 drop / s. After the addition was completed, the mixture was heated to 45° C. and the stirring reaction was continued for 10 h. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed twice with distilled water, and then placed in a vacuum drying oven and dried at a temperature of 55° C. for 2 h to obtain an inorganic multi-effect flame retardant. Step A5: 2 g of an organic multi-effect flame retardant, 40 mL of anhydrous ethanol and 5 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred for reaction at a temperature of 20° C. and a stirring rate of 300 r / min for 15 min, and then the pH was adjusted to 2 with anhydrous acetic acid, and then the stirring reaction was continued for 5 min. Then, 5 g of an inorganic multi-effect flame retardant was added and the mixture was stirred for reaction for 5 h under the condition of heating to 75° C. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed twice with distilled water, and then placed in a vacuum drying oven and dried at a temperature of 55° C. for 2 h to obtain a composite flame retardant; Step A6: weigh 76 parts of polyester resin and 4.8 parts of composite flame retardant according to weight; the model of the polyester resin is JT-B1; Step A7: the polyester resin and the composite flame retardant are mixed evenly, and then melt-extruded through a twin-screw extruder, cooled, pelletized, and then melt-spun to obtain flame-retardant polyester fibers; Step A8: blending the flame-retardant polyester fiber and the cotton fiber in a mass ratio of 65:35 to obtain a polyester-cotton yarn; Step A9: Weaving the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0016] Embodiment 2: This embodiment is a preparation process of a halogen-free flame-retardant polyester-cotton fabric, comprising the following steps: Step A1: 10 mmol melamine, 30 mmol terephthalaldehyde, 0.10 g anhydrous sodium acetate and 52 mL anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen was introduced for protection. The mixture was stirred for reaction at a temperature of 22° C. and a stirring rate of 350 r / min for 20 min, and then the temperature was raised to reflux and the stirring reaction was continued for 4.5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 1; Step A2: 10 mmol of intermediate 1, 30 mmol of 3-aminopropyltriethoxysilane, 0.12 g of anhydrous sodium acetate and 65 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 22° C. and a stirring rate of 350 r / min for 25 min, and then the temperature was raised to 82° C. and the stirring reaction was continued for 6.5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 2; Step A3: 10 mmol of intermediate 2, 60 mmol of DOPO and 110 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The reaction was stirred at 82° C. and a stirring rate of 350 r / min for 18 min, and then the temperature was raised to 105° C. and the stirring reaction was continued for 11 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation, and then added to ice water, and then allowed to stand to precipitate, and then vacuum filtered. The filter cake was placed in a vacuum drying oven and dried at 62° C. for 2.5 h to obtain an organic multi-effect flame retardant; Step A4: 12 g of anhydrous magnesium sulfate and 48 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and the mixture was stirred for 18 min at a temperature of 22 ° C and a stirring rate of 350 r / min, and then 3 g of activated carbon and 0.4 g of sodium dodecylbenzene sulfonate were added and the stirring reaction was continued for 18 min, and then 20 mL of 22% ammonia water was added dropwise while stirring, and the dropping rate was controlled to be 1 drop / s. After the addition was completed, the mixture was heated to 50 ° C and the stirring reaction was continued for 12 h. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed twice with distilled water, and then placed in a vacuum drying oven and dried at a temperature of 58 ° C for 2.5 h to obtain an inorganic multi-effect flame retardant; Step A5: 6 g of an organic multi-effect flame retardant, 42 mL of anhydrous ethanol and 7 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred for reaction at a temperature of 22° C. and a stirring rate of 350 r / min for 18 min, and then the pH was adjusted to 2.5 with anhydrous acetic acid, and then the stirring reaction was continued for 7 min. Then, 5 g of an inorganic multi-effect flame retardant was added and the mixture was stirred for reaction for 5.5 h under the condition of heating to 78° C. After the reaction, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed twice with distilled water, and then placed in a vacuum drying oven and dried at a temperature of 58° C. for 2.5 h to obtain a composite flame retardant; Step A6: Weigh 79 parts of polyester resin and 8.5 parts of composite flame retardant according to weight; the model of the polyester resin is JT-B1; Step A7: the polyester resin and the composite flame retardant are mixed evenly, and then melt-extruded through a twin-screw extruder, cooled, pelletized, and then melt-spun to obtain flame-retardant polyester fibers; Step A8: blending the flame-retardant polyester fiber and the cotton fiber in a mass ratio of 65:35 to obtain a polyester-cotton yarn; Step A9: Weaving the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0017] Embodiment 3: This embodiment is a preparation process of a halogen-free flame-retardant polyester-cotton fabric, comprising the following steps: Step A1: 10 mmol melamine, 30 mmol terephthalaldehyde, 0.15 g anhydrous sodium acetate and 55 mL anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 25° C. and a stirring rate of 400 r / min for 25 min, and then the temperature was raised to reflux and the stirring reaction was continued for 5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 1; Step A2: 10 mmol of intermediate 1, 30 mmol of 3-aminopropyltriethoxysilane, 0.16 g of anhydrous sodium acetate and 70 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at 25° C. and a stirring rate of 400 r / min for 30 min, and then the temperature was raised to 85° C. and the stirring reaction was continued for 7 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 2; Step A3: 10 mmol of intermediate 2, 60 mmol of DOPO and 120 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred at 85° C. and a stirring rate of 400 r / min for 20 min, and then the mixture was heated to 110° C. and the stirring reaction was continued for 12 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The product was then added to ice water, and then allowed to stand to precipitate. The product was then vacuum filtered, and the filter cake was placed in a vacuum drying oven and dried at 65° C. for 3 h to obtain an organic multi-effect flame retardant. Step A4: 15 g of anhydrous magnesium sulfate and 50 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and the mixture was stirred for reaction at a temperature of 25° C. and a stirring rate of 400 r / min for 20 min. Then, 3 g of activated carbon and 0.6 g of sodium dodecylbenzene sulfonate were added and the stirring reaction was continued for 20 min. Then, 25 mL of 25% ammonia water was added dropwise while stirring, and the dropping rate was controlled to be 2 drops / s. After the addition was completed, the mixture was heated to 55° C. and the stirring reaction was continued for 15 h. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with distilled water 3 times, and then placed in a vacuum drying oven and dried at a temperature of 60° C. for 3 h to obtain an inorganic multi-effect flame retardant. Step A5: 10 g of an organic multi-effect flame retardant, 45 mL of anhydrous ethanol and 10 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred for reaction at a temperature of 25° C. and a stirring rate of 400 r / min for 20 min, and then the pH was adjusted to 3 with anhydrous acetic acid, and then the stirring reaction was continued for 10 min. Then, 5 g of an inorganic multi-effect flame retardant was added and the mixture was stirred for reaction for 6 h under the condition of heating to 80° C. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed 3 times with distilled water, and then placed in a vacuum drying oven and dried at a temperature of 60° C. for 3 h to obtain a composite flame retardant; Step A6: Weigh 82 parts of polyester resin and 12.2 parts of composite flame retardant according to weight; the model of the polyester resin is JT-B1; Step A7: the polyester resin and the composite flame retardant are mixed evenly, and then melt-extruded through a twin-screw extruder, cooled, pelletized, and then melt-spun to obtain flame-retardant polyester fibers; Step A8: blending the flame-retardant polyester fiber and the cotton fiber in a mass ratio of 65:35 to obtain a polyester-cotton yarn; Step A9: Weaving the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0018] Comparative Example 1: This comparative example is a preparation process of a halogen-free flame-retardant polyester-cotton fabric, comprising the following steps: Step A1: weigh 82 parts of polyester resin according to weight; the model of the polyester resin is JT-B1; Step A2: the polyester resin and the composite flame retardant are mixed evenly, and then melt-extruded through a twin-screw extruder, cooled, pelletized, and then melt-spun to obtain flame-retardant polyester fibers; Step A3: blending the flame-retardant polyester fiber and the cotton fiber in a mass ratio of 65:35 to obtain a polyester-cotton yarn; Step A4: Weaving the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0019] Comparative Example 2: This comparative example is a preparation process of a halogen-free flame-retardant polyester-cotton fabric, comprising the following steps: Step A1: 10 mmol melamine, 30 mmol terephthalaldehyde, 0.15 g anhydrous sodium acetate and 55 mL anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 25° C. and a stirring rate of 400 r / min for 25 min, and then the temperature was raised to reflux and the stirring reaction was continued for 5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 1; Step A2: 10 mmol of intermediate 1, 30 mmol of 3-aminopropyltriethoxysilane, 0.16 g of anhydrous sodium acetate and 70 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at 25° C. and a stirring rate of 400 r / min for 30 min, and then the temperature was raised to 85° C. and the stirring reaction was continued for 7 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 2; Step A3: 10 mmol of intermediate 2, 60 mmol of DOPO and 120 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred at 85° C. and a stirring rate of 400 r / min for 20 min, and then the mixture was heated to 110° C. and the stirring reaction was continued for 12 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The product was then added to ice water, and then allowed to stand to precipitate. The product was then vacuum filtered, and the filter cake was placed in a vacuum drying oven and dried at 65° C. for 3 h to obtain an organic multi-effect flame retardant. Step A4: weigh 82 parts of polyester resin and 12.2 parts of organic multi-effect flame retardant according to weight; the model of the polyester resin is JT-B1; Step A5: the polyester resin and the composite flame retardant are mixed evenly, and then melt-extruded through a twin-screw extruder, cooled, pelletized, and then melt-spun to obtain flame-retardant polyester fibers; Step A6: blending the flame-retardant polyester fiber and the cotton fiber in a mass ratio of 65:35 to obtain a polyester-cotton yarn; Step A7: Weaving the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0020] Comparative Example 3: This comparative example is a preparation process of a halogen-free flame-retardant polyester-cotton fabric, comprising the following steps: Step A1: 15 g of anhydrous magnesium sulfate and 50 mL of deionized water are added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and the mixture is stirred for reaction at a temperature of 25° C. and a stirring rate of 400 r / min for 20 min, and then 3 g of activated carbon and 0.6 g of sodium dodecylbenzene sulfonate are added and the stirring reaction is continued for 20 min, and then 25 mL of 25% ammonia water by mass is added dropwise while stirring, and the dropping rate is controlled to be 2 drops / s. After the dropwise addition is completed, the mixture is heated to 55° C. and the stirring reaction is continued for 15 h. After the reaction is completed, the reaction product is cooled to room temperature and then centrifuged. The precipitate is washed 3 times with distilled water, and then placed in a vacuum drying oven and dried at a temperature of 60° C. for 3 h to obtain an inorganic multi-effect flame retardant; Step A2: Weigh 82 parts of polyester resin and 12.2 parts of inorganic multi-effect flame retardant according to weight; the model of the polyester resin is JT-B1; Step A3: the polyester resin and the composite flame retardant are mixed evenly, and then melt-extruded through a twin-screw extruder, cooled, pelletized, and then melt-spun to obtain flame-retardant polyester fibers; Step A4: blending the flame-retardant polyester fiber and the cotton fiber in a mass ratio of 65:35 to obtain a polyester-cotton yarn; Step A5: Weaving the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0021] The halogen-free flame-retardant polyester-cotton fabrics of Examples 1-3 and Comparative Examples 1-3 were subjected to performance tests, and the test results are shown in the following table:

[0022] Referring to the data in the above table, according to the comparison between Examples 1-3 and Comparative Examples 1-3, it can be seen that the addition of organic multi-effect flame retardants, inorganic multi-effect flame retardants and composite flame retardants can significantly improve the flame retardant properties of polyester-cotton fabrics, among which the composite flame retardant has the best effect on improving the flame retardant properties of polyester-cotton fabrics, so that the prepared polyester-cotton fabrics have excellent flame retardant properties.

[0023] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0024] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.

Claims

1. A preparation process of a halogen-free flame-retardant polyester-cotton fabric, characterized in that: The following steps are involved: Step 1: Weigh 76-82 parts of polyester resin and 4.8-12.2 parts of composite flame retardant according to weight; the model of the polyester resin is JT-B1; Step 2: Evenly mix the polyester resin and the composite flame retardant, and then melt extrude the mixture through a twin-screw extruder, cool and pelletize the mixture, and then melt spin the mixture to obtain a flame-retardant polyester fiber; Step 3: blending the flame retardant polyester fiber and the cotton fiber in a mass ratio of 65:35 to obtain polyester-cotton yarn; Step 4: Weaving the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric; Wherein, the composite flame retardant is prepared by the following steps: Step s1: stirring melamine, terephthalaldehyde, anhydrous sodium acetate and anhydrous ethanol for reaction, cooling the reaction product after the reaction is completed, and then rotary evaporating to obtain intermediate 1; Step s2: stirring the intermediate 1, 3-aminopropyltriethoxysilane, anhydrous sodium acetate and anhydrous ethanol to react, cooling the reaction product after the reaction is completed, and then rotary evaporating to obtain the intermediate 2; Step s3: stirring the intermediate 2, DOPO and anhydrous ethanol for reaction, cooling the reaction product after the reaction is completed, then rotary evaporating, then adding it into ice water, then standing to precipitate, then vacuum filtering, and drying the filter cake to obtain an organic multi-effect flame retardant; Step s4: stirring anhydrous magnesium sulfate and deionized water for reaction, then adding activated carbon and sodium dodecylbenzene sulfonate and continuing to stir the reaction, then adding ammonia water dropwise while stirring, and continuing to stir the reaction after the dropwise addition is completed. After the reaction is completed, the reaction product is cooled, then centrifuged, and the precipitate is washed and dried to obtain an inorganic multi-effect flame retardant; Step s5: Stir the organic multi-effect flame retardant, anhydrous ethanol and deionized water for reaction, then adjust the pH with anhydrous acetic acid, continue to stir the reaction, then add the inorganic multi-effect flame retardant and continue to stir the reaction. After the reaction is completed, cool the reaction product, then centrifuge it, wash and dry the precipitate to obtain a composite flame retardant.

2. The preparation process of a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that: The usage ratio of melamine, terephthalaldehyde, anhydrous sodium acetate and anhydrous ethanol in step s1 is 10mmol:30mmol:0.05-0.15g:50-55mL.

3. The preparation process of a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that: The usage ratio of the intermediate 1, 3-aminopropyltriethoxysilane, anhydrous sodium acetate and anhydrous ethanol in step s2 is 10 mmol: 30 mmol: 0.08-0.16 g: 60-70 mL.

4. The preparation process of a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that: The usage ratio of the intermediate 2, DOPO and anhydrous ethanol in step s3 is 10 mmol: 60 mmol: 100-120 mL.

5. The preparation process of a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that: The dosage ratio of the anhydrous magnesium sulfate, deionized water, activated carbon, sodium dodecylbenzene sulfonate and ammonia water in step s4 is 10-15g:45-50mL:3g:0.2-0.6g:15-25mL.

6. The process for preparing a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that: The mass fraction of the ammonia water in step s4 is 20-25%.

7. The process for preparing a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that: The usage ratio of the organic multi-effect flame retardant, anhydrous ethanol, deionized water and inorganic multi-effect flame retardant in step s5 is 2-10g:40-45mL:5-10mL:5g.

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