A preparation process for halogen-free flame-retardant polyester-cotton fabric

Abstract

This invention relates to the field of textile materials, specifically to a preparation process for halogen-free flame-retardant polyester-cotton fabric. This process addresses the problems of poor flame-retardant performance in existing polyester-cotton fabrics and the fact that most flame-retardant fabrics are treated with halogen-containing compounds, which can easily cause harm to the environment and human health. This invention uses a halogen-free flame retardant, avoiding the problem of toxic gases produced during combustion by traditional halogen-containing flame retardants, thus meeting environmental protection requirements. By producing flame-retardant polyester fibers for blending, the fabric possesses excellent flame-retardant properties, making it suitable for applications such as power protective clothing and fire-fighting suits. Furthermore, the preparation process of this invention is relatively simple, easy to industrialize, and reduces production costs.

Description

Technical Field

[0001] This invention relates to the field of textile materials, specifically to a preparation process for halogen-free flame-retardant polyester-cotton fabric. Background Technology

[0002] Polyester-cotton blend refers to a general term for blended fabrics made from polyester and cotton yarns. Commonly known as "Dacron," it retains the high strength and good elasticity of polyester fibers while also possessing the high moisture absorption of cotton fibers. It is easy to dye, requires no ironing, and dries quickly, making it a common material for clothing production. Its applications, especially in apparel, are very extensive, and the market is huge.

[0003] With the increasing demand for protective clothing in fields such as firefighting, power, and the military, higher requirements are being placed on the flame-retardant properties of textile fabrics. Traditional polyester-cotton fabrics are easily ignited when exposed to a fire source, posing a safety hazard. Currently, most flame-retardant fabrics on the market are treated with halogen-containing compounds, but these compounds produce toxic gases when burned, harming the environment and human health. Therefore, developing an environmentally friendly and highly efficient halogen-free flame-retardant polyester-cotton fabric is of significant practical importance. Summary of the Invention

[0004] In order to overcome the above-mentioned technical problems, the purpose of this invention is to provide a preparation process for halogen-free flame-retardant polyester-cotton fabric, which solves the problems that existing polyester-cotton fabrics have poor flame-retardant performance and that flame-retardant fabrics are mostly treated with halogen-containing compounds, which can easily cause harm to the environment and human health.

[0005] The objective of this invention can be achieved through the following technical solutions:

[0006] A process for preparing a halogen-free flame-retardant polyester-cotton fabric includes the following steps:

[0007] Step 1: Weigh out 76-82 parts of polyester resin and 4.8-12.2 parts of composite flame retardant according to the following weight proportions; the polyester resin is of type JT-B1.

[0008] Step 2: Mix polyester resin and composite flame retardant evenly, then melt-extrude through a twin-screw extruder, cool and pelletize, and then melt-spin to obtain flame-retardant polyester fiber;

[0009] Step 3: Blend flame-retardant polyester fiber and cotton fiber at a mass ratio of 65:35 to obtain polyester-cotton yarn;

[0010] Step 4: Weave the polyester-cotton yarn into a polyester-cotton fabric to obtain halogen-free flame-retardant polyester-cotton fabric.

[0011] As a further aspect of the present invention: the composite flame retardant is prepared by the following steps:

[0012] Step s1: Melamine, terephthalaldehyde, anhydrous sodium acetate and anhydrous ethanol are added to a three-necked flask equipped with a stirrer, thermometer, gas delivery tube and reflux condenser. Nitrogen gas is introduced for protection. The mixture is stirred for 15-25 min at a temperature of 20-25℃ and a stirring rate of 300-400 r / min. Then the temperature is raised to reflux and the mixture is stirred for 4-5 h. After the reaction is completed, the reaction product is cooled to room temperature and the solvent is removed by rotary evaporation to obtain intermediate 1.

[0013] Step s2: Add intermediate 1, 3-aminopropyltriethoxysilane, anhydrous sodium acetate and anhydrous ethanol to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen for protection and stir the reaction at 20-25℃ and 300-400 r / min for 20-30 min. Then raise the temperature to 80-85℃ and continue stirring for 6-7 h. After the reaction is completed, cool the reaction product to room temperature and then remove the solvent by rotary evaporation to obtain intermediate 2.

[0014] Step s3: Add intermediate 2, DOPO and anhydrous ethanol to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen for protection. Stir and react for 15-20 min at 80-85℃ and 300-400 r / min. Then raise the temperature to 100-110℃ and continue stirring for 10-12 h. After the reaction is complete, cool the reaction product to room temperature, then remove the solvent by rotary evaporation, 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 for 2-3 h at 60-65℃ to obtain the organic multi-effect flame retardant.

[0015] Step s4: Add anhydrous magnesium sulfate and deionized water to a three-necked flask equipped with a stirrer, thermometer, and constant pressure dropping funnel. Stir the reaction for 15-20 min at a temperature of 20-25℃ and a stirring rate of 300-400 r / min. Then add activated carbon and sodium dodecylbenzenesulfonate and continue stirring for another 15-20 min. Then add ammonia water dropwise while stirring, controlling the dropping rate to 1-2 drops / s. After the addition is complete, raise the temperature to 45-55℃ and continue stirring for 10-15 h. After the reaction is complete, cool the reaction product to room temperature, then centrifuge. Wash the precipitate 2-3 times with distilled water, then place it in a vacuum drying oven and dry it for 2-3 h at a temperature of 55-60℃ to obtain the inorganic multi-effect flame retardant.

[0016] Step s5: Add the organic multi-effect flame retardant, anhydrous ethanol, and deionized water to a three-necked flask equipped with a stirrer, thermometer, and gas delivery tube. Purge with nitrogen for protection and stir for 15-20 minutes at a temperature of 20-25℃ and a stirring rate of 300-400 r / min. Then adjust the pH to 2-3 with anhydrous acetic acid and continue stirring for 5-10 minutes. Add the inorganic multi-effect flame retardant and continue stirring for 5-6 hours at a temperature of 75-80℃. After the reaction is complete, cool the reaction product to room temperature, centrifuge, wash the precipitate 2-3 times with distilled water, and then place it in a vacuum drying oven and dry at a temperature of 55-60℃ for 2-3 hours to obtain the composite flame retardant.

[0017] As a further aspect of the present invention: the 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.

[0018] As a further aspect of the present invention: the ratio of 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.

[0019] As a further aspect of the present invention: the ratio of intermediate 2, DOPO and anhydrous ethanol in step s3 is 10 mmol: 60 mmol: 100-120 mL.

[0020] As a further aspect of the present invention: the ratio of anhydrous magnesium sulfate, deionized water, activated carbon, sodium dodecylbenzenesulfonate and ammonia in step s4 is 10-15g: 45-50mL: 3g: 0.2-0.6g: 15-25mL.

[0021] As a further aspect of the present invention: the mass fraction of the ammonia water in step s4 is 20-25%.

[0022] As a further aspect of the present invention: the 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.

[0023] The beneficial effects of this invention are:

[0024] This invention discloses a process for preparing halogen-free flame-retardant polyester-cotton fabric. The process involves uniformly mixing polyester resin and a composite flame retardant, followed by melt extrusion, cooling, pelletizing, and then melt spinning to obtain flame-retardant polyester fibers. These flame-retardant polyester fibers are then blended with cotton fibers to obtain polyester-cotton yarn. Finally, the polyester-cotton yarn is woven into a polyester-cotton fabric to obtain the halogen-free flame-retardant polyester-cotton fabric. This invention uses a halogen-free flame retardant, avoiding the problem of toxic gases produced during combustion by traditional halogen-containing flame retardants, thus meeting environmental protection requirements. By producing flame-retardant polyester fibers for blending, the fabric possesses excellent flame-retardant properties, making it suitable for applications such as power protective clothing and fire-fighting suits. Furthermore, the preparation process of this invention is relatively simple, easy to industrialize, and reduces production costs.

[0025] In the preparation of halogen-free flame-retardant polyester-cotton fabric, a composite flame retardant was first prepared. This involved the reaction of melamine and terephthalaldehyde. The amino group on melamine reacted with an aldehyde group on terephthalaldehyde via a Schiff base reaction, forming a C=N bond and introducing an aldehyde group, yielding intermediate 1. Next, intermediate 1 reacted with 3-aminopropyltriethoxysilane. The aldehyde group on intermediate 1 reacted with the amino group on 3-aminopropyltriethoxysilane via a Schiff base reaction, forming a C=N bond and introducing a large number of siloxane groups, yielding intermediate 2. The intermediates were then... 2. The DOPO reaction involves the C=N bond on intermediate 2 reacting with the PH bond on DOPO to introduce an organophosphorus compound, yielding an organic multi-functional flame retardant. Subsequently, anhydrous magnesium sulfate, ammonia, and activated carbon react to form magnesium hydroxide on the surface of the activated carbon, creating a composite structure of magnesium hydroxide encapsulating the activated carbon, resulting in an inorganic multi-functional flame retardant. This inorganic multi-functional flame retardant is then treated with the organic multi-functional flame retardant. The siloxane groups on the organic multi-functional flame retardant hydrolyze to form silanols, which, after dehydration and condensation, can be grafted onto the particle surface of the inorganic multi-functional flame retardant. A composite flame retardant was obtained. The activated carbon in this composite flame retardant has an extremely high surface area and uniform pore size distribution, which enables it to effectively adsorb organic matter, impurities, and combustible gases. It also forms a carbon layer on the material surface, which can prevent the matrix from direct contact with air, thus achieving a flame retardant effect. Subsequently, the magnesium hydroxide coated on the activated carbon surface can absorb a large amount of heat during thermal decomposition, while generating a large amount of water vapor and high-temperature resistant metal oxides to exert a flame retardant effect. The organic multi-effect flame retardant grafted on the magnesium hydroxide surface can effectively improve the dispersibility of the composite flame retardant, allowing it to be uniformly dispersed in the flame-retardant polyester fiber, achieving an excellent flame retardant effect. Moreover, the organic multi-effect flame retardant contains a large amount of organic phosphorus and organic nitrogen in its molecular structure. Under the synergistic effect of the two, it can reduce the concentration of combustible gases and promote the formation of the carbon layer, thereby effectively preventing the spread of flames and achieving a flame retardant effect. Therefore, under the synergistic effect of the organic and inorganic multi-effect flame retardants, the composite flame retardant is endowed with a high flame retardant effect, resulting in excellent flame retardant properties of the prepared polyester-cotton fabric. Detailed Implementation

[0026] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0027] Example 1:

[0028] This embodiment describes a preparation process for a halogen-free flame-retardant polyester-cotton fabric, including the following steps:

[0029] Step A1: 10 mmol of melamine, 30 mmol of terephthalaldehyde, 0.05 g of anhydrous sodium acetate and 50 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, thermometer, gas delivery tube and reflux condenser. Nitrogen gas was introduced for protection. The mixture was stirred at 20 °C and 300 r / min for 15 min. Then the temperature was raised to reflux and the mixture was stirred for 4 h. After the reaction was completed, the reaction product was cooled to room temperature and the solvent was removed by rotary evaporation to obtain intermediate 1.

[0030] 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, thermometer and gas delivery tube. Nitrogen gas was introduced for protection. The mixture was stirred at 20 °C and 300 r / min for 20 min. Then the temperature was raised to 80 °C and the mixture was stirred for 6 h. After the reaction was completed, the reaction product was cooled to room temperature and the solvent was removed by rotary evaporation to obtain intermediate 2.

[0031] Step A3: Add 10 mmol of intermediate 2, 60 mmol of DOPO and 100 mL of anhydrous ethanol to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen for protection and stir at 80 °C and 300 r / min for 15 min. Then raise the temperature to 100 °C and continue stirring for 10 h. After the reaction is complete, cool the reaction product to room temperature, remove the solvent by rotary evaporation, add it to ice water, let it stand to precipitate, then vacuum filter it. Place the filter cake in a vacuum drying oven and dry it at 60 °C for 2 h to obtain the organic multi-effect flame retardant.

[0032] Step A4: Add 10g of anhydrous magnesium sulfate and 45mL of deionized water to a three-necked flask equipped with a stirrer, thermometer, and constant pressure dropping funnel. Stir the reaction at 20℃ and a stirring rate of 300r / min for 15min. Then add 3g of activated carbon and 0.2g of sodium dodecylbenzenesulfonate and continue stirring for 15min. Then add 15mL of 20% ammonia water dropwise while stirring, controlling the dropping rate to 1 drop / s. After the addition is complete, raise the temperature to 45℃ and continue stirring for 10h. After the reaction is complete, cool the reaction product to room temperature, then centrifuge. Wash the precipitate twice with distilled water and then place it in a vacuum drying oven at 55℃ for 2h to obtain the inorganic multi-effect flame retardant.

[0033] Step A5: Add 2g of organic multi-effect flame retardant, 40mL of anhydrous ethanol and 5mL of deionized water to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen for protection and stir for 15min at 20℃ and 300r / min. Then adjust the pH to 2 with anhydrous acetic acid and continue stirring for 5min. Then add 5g of inorganic multi-effect flame retardant and continue stirring for 5h at 75℃. After the reaction is complete, cool the reaction product to room temperature, then centrifuge. Wash the precipitate twice with distilled water and then place it in a vacuum drying oven and dry at 55℃ for 2h to obtain the composite flame retardant.

[0034] Step A6: Weigh out 76 parts of polyester resin and 4.8 parts of composite flame retardant according to the following weight proportions; the polyester resin is of type JT-B1;

[0035] Step A7: Mix polyester resin and composite flame retardant evenly, then melt extrude through a twin-screw extruder, cool and pelletize, and then melt spin to obtain flame-retardant polyester fiber;

[0036] Step A8: Blend flame-retardant polyester fiber and cotton fiber at a mass ratio of 65:35 to obtain polyester-cotton yarn;

[0037] Step A9: Weave the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0038] Example 2:

[0039] This embodiment describes a preparation process for a halogen-free flame-retardant polyester-cotton fabric, including the following steps:

[0040] Step A1: 10 mmol of melamine, 30 mmol of terephthalaldehyde, 0.10 g of anhydrous sodium acetate and 52 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, thermometer, gas delivery tube and reflux condenser. Nitrogen gas was introduced for protection. The mixture was stirred at 22 °C and 350 r / min for 20 min. Then the temperature was raised to reflux and the mixture was stirred for another 4.5 h. After the reaction was completed, the reaction product was cooled to room temperature and the solvent was removed by rotary evaporation to obtain intermediate 1.

[0041] 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, thermometer and gas delivery tube. Nitrogen gas was introduced for protection, and the mixture was stirred at 22 °C and 350 r / min for 25 min. Then the temperature was raised to 82 °C and the mixture was stirred for 6.5 h. After the reaction was completed, the reaction product was cooled to room temperature and the solvent was removed by rotary evaporation to obtain intermediate 2.

[0042] Step A3: Add 10 mmol of intermediate 2, 60 mmol of DOPO and 110 mL of anhydrous ethanol to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen for protection and stir at 82 °C and 350 r / min for 18 min. Then raise the temperature to 105 °C and continue stirring for 11 h. After the reaction is complete, cool the reaction product to room temperature, remove the solvent by rotary evaporation, add it to ice water, let it stand to precipitate, then vacuum filter it. Place the filter cake in a vacuum drying oven and dry it at 62 °C for 2.5 h to obtain the organic multi-effect flame retardant.

[0043] Step A4: Add 12g of anhydrous magnesium sulfate and 48mL of deionized water to a three-necked flask equipped with a stirrer, thermometer, and constant pressure dropping funnel. Stir the mixture at 22℃ and a stirring rate of 350r / min for 18min. Then add 3g of activated carbon and 0.4g of sodium dodecylbenzenesulfonate and continue stirring for another 18min. Then, while stirring, add 20mL of 22% ammonia water dropwise at a rate of 1 drop / s. After the addition is complete, raise the temperature to 50℃ and continue stirring for 12h. After the reaction is complete, cool the reaction product to room temperature, centrifuge, wash the precipitate twice with distilled water, and then place it in a vacuum drying oven and dry it at 58℃ for 2.5h to obtain the inorganic multi-effect flame retardant.

[0044] Step A5: Add 6g of organic multi-effect flame retardant, 42mL of anhydrous ethanol and 7mL of deionized water to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen for protection and stir at 22℃ and 350r / min for 18min. Then adjust the pH to 2.5 with anhydrous acetic acid and continue stirring for 7min. Then add 5g of inorganic multi-effect flame retardant and heat to 78℃ and continue stirring for 5.5h. After the reaction is complete, cool the reaction product to room temperature, centrifuge, wash the precipitate twice with distilled water, and then place it in a vacuum drying oven and dry at 58℃ for 2.5h to obtain the composite flame retardant.

[0045] Step A6: Weigh out 79 parts of polyester resin and 8.5 parts of composite flame retardant according to the following weight proportions; the polyester resin is of type JT-B1;

[0046] Step A7: Mix polyester resin and composite flame retardant evenly, then melt extrude through a twin-screw extruder, cool and pelletize, and then melt spin to obtain flame-retardant polyester fiber;

[0047] Step A8: Blend flame-retardant polyester fiber and cotton fiber at a mass ratio of 65:35 to obtain polyester-cotton yarn;

[0048] Step A9: Weave the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0049] Example 3:

[0050] This embodiment describes a preparation process for a halogen-free flame-retardant polyester-cotton fabric, including the following steps:

[0051] Step A1: 10 mmol of melamine, 30 mmol of terephthalaldehyde, 0.15 g of anhydrous sodium acetate and 55 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, thermometer, gas delivery tube and reflux condenser. Nitrogen gas was introduced for protection. The mixture was stirred at 25 °C and 400 r / min for 25 min. Then the temperature was raised to reflux and the mixture was stirred for another 5 h. After the reaction was completed, the reaction product was cooled to room temperature and the solvent was removed by rotary evaporation to obtain intermediate 1.

[0052] 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, thermometer and gas delivery tube. Nitrogen gas was introduced for protection. The mixture was stirred at 25 °C and 400 r / min for 30 min. Then the temperature was raised to 85 °C and the mixture was stirred for 7 h. After the reaction was completed, the product was cooled to room temperature and the solvent was removed by rotary evaporation to obtain intermediate 2.

[0053] Step A3: Add 10 mmol of intermediate 2, 60 mmol of DOPO and 120 mL of anhydrous ethanol to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen and stir at 85 °C and 400 r / min for 20 min. Then raise the temperature to 110 °C and continue stirring for 12 h. After the reaction is complete, cool the reaction product to room temperature, remove the solvent by rotary evaporation, add it to ice water, let it stand to precipitate, then vacuum filter it. Place the filter cake in a vacuum drying oven and dry it at 65 °C for 3 h to obtain the organic multi-effect flame retardant.

[0054] Step A4: Add 15g of anhydrous magnesium sulfate and 50mL of deionized water to a three-necked flask equipped with a stirrer, thermometer, and constant pressure dropping funnel. Stir the reaction for 20min at 25℃ and a stirring rate of 400r / min. Then add 3g of activated carbon and 0.6g of sodium dodecylbenzenesulfonate and continue stirring for another 20min. Then add 25mL of 25% ammonia water dropwise while stirring, controlling the dropping rate to 2 drops / s. After the addition is complete, raise the temperature to 55℃ and continue stirring for 15h. After the reaction is complete, cool the reaction product to room temperature, then centrifuge. Wash the precipitate three times with distilled water and then place it in a vacuum drying oven at 60℃ for 3h to obtain the inorganic multi-effect flame retardant.

[0055] Step A5: Add 10g of organic multi-effect flame retardant, 45mL of anhydrous ethanol and 10mL of deionized water to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen for protection and stir at 25℃ and 400r / min for 20min. Then adjust the pH to 3 with anhydrous acetic acid and continue stirring for 10min. Then add 5g of inorganic multi-effect flame retardant and heat to 80℃ and continue stirring for 6h. After the reaction is complete, cool the reaction product to room temperature, then centrifuge. Wash the precipitate three times with distilled water and then place it in a vacuum drying oven and dry at 60℃ for 3h to obtain the composite flame retardant.

[0056] Step A6: Weigh out 82 parts of polyester resin and 12.2 parts of composite flame retardant according to the following weight proportions; the polyester resin is of type JT-B1;

[0057] Step A7: Mix polyester resin and composite flame retardant evenly, then melt extrude through a twin-screw extruder, cool and pelletize, and then melt spin to obtain flame-retardant polyester fiber;

[0058] Step A8: Blend flame-retardant polyester fiber and cotton fiber at a mass ratio of 65:35 to obtain polyester-cotton yarn;

[0059] Step A9: Weave the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0060] Comparative Example 1:

[0061] This comparative example illustrates a preparation process for a halogen-free flame-retardant polyester-cotton fabric, including the following steps:

[0062] Step A1: Weigh 82 parts of polyester resin according to the specified weight; the polyester resin is of type JT-B1.

[0063] Step A2: Mix polyester resin and composite flame retardant evenly, then melt-extrude through a twin-screw extruder, cool and pelletize, and then melt-spin to obtain flame-retardant polyester fiber;

[0064] Step A3: Blend flame-retardant polyester fiber and cotton fiber at a mass ratio of 65:35 to obtain polyester-cotton yarn;

[0065] Step A4: Weave the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0066] Comparative Example 2:

[0067] This comparative example illustrates a preparation process for a halogen-free flame-retardant polyester-cotton fabric, including the following steps:

[0068] Step A1: 10 mmol of melamine, 30 mmol of terephthalaldehyde, 0.15 g of anhydrous sodium acetate and 55 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, thermometer, gas delivery tube and reflux condenser. Nitrogen gas was introduced for protection. The mixture was stirred at 25 °C and 400 r / min for 25 min. Then the temperature was raised to reflux and the mixture was stirred for another 5 h. After the reaction was completed, the reaction product was cooled to room temperature and the solvent was removed by rotary evaporation to obtain intermediate 1.

[0069] 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, thermometer and gas delivery tube. Nitrogen gas was introduced for protection. The mixture was stirred at 25 °C and 400 r / min for 30 min. Then the temperature was raised to 85 °C and the mixture was stirred for 7 h. After the reaction was completed, the product was cooled to room temperature and the solvent was removed by rotary evaporation to obtain intermediate 2.

[0070] Step A3: Add 10 mmol of intermediate 2, 60 mmol of DOPO and 120 mL of anhydrous ethanol to a three-necked flask equipped with a stirrer, thermometer and gas delivery tube. Purge with nitrogen and stir at 85 °C and 400 r / min for 20 min. Then raise the temperature to 110 °C and continue stirring for 12 h. After the reaction is complete, cool the reaction product to room temperature, remove the solvent by rotary evaporation, add it to ice water, let it stand to precipitate, then vacuum filter it. Place the filter cake in a vacuum drying oven and dry it at 65 °C for 3 h to obtain the organic multi-effect flame retardant.

[0071] Step A4: Weigh out 82 parts of polyester resin and 12.2 parts of organic multi-effect flame retardant according to the following weight proportions; the polyester resin is of type JT-B1;

[0072] Step A5: Mix polyester resin and composite flame retardant evenly, then melt-extrude through a twin-screw extruder, cool and pelletize, and then melt-spin to obtain flame-retardant polyester fiber;

[0073] Step A6: Blend flame-retardant polyester fiber and cotton fiber at a mass ratio of 65:35 to obtain polyester-cotton yarn;

[0074] Step A7: Weave the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0075] Comparative Example 3:

[0076] This comparative example illustrates a preparation process for a halogen-free flame-retardant polyester-cotton fabric, including the following steps:

[0077] Step A1: Add 15g of anhydrous magnesium sulfate and 50mL of deionized water to a three-necked flask equipped with a stirrer, thermometer, and constant pressure dropping funnel. Stir the reaction at 25℃ and 400r / min for 20min. Then add 3g of activated carbon and 0.6g of sodium dodecylbenzenesulfonate and continue stirring for another 20min. Then add 25mL of 25% ammonia water dropwise while stirring, controlling the dropping rate to 2 drops / s. After the addition is complete, raise the temperature to 55℃ and continue stirring for 15h. After the reaction is complete, cool the reaction product to room temperature, then centrifuge. Wash the precipitate three times with distilled water and then place it in a vacuum drying oven at 60℃ for 3h to obtain the inorganic multi-effect flame retardant.

[0078] Step A2: Weigh out 82 parts by weight of polyester resin and 12.2 parts by weight of inorganic multi-effect flame retardant; the polyester resin is of type JT-B1;

[0079] Step A3: Mix polyester resin and composite flame retardant evenly, then melt extrude through a twin-screw extruder, cool and pelletize, and then melt spin to obtain flame-retardant polyester fiber;

[0080] Step A4: Blend flame-retardant polyester fiber and cotton fiber at a mass ratio of 65:35 to obtain polyester-cotton yarn;

[0081] Step A5: Weave the polyester-cotton yarn into a polyester-cotton fabric to obtain a halogen-free flame-retardant polyester-cotton fabric.

[0082] The performance of the halogen-free flame-retardant polyester-cotton fabrics from Examples 1-3 and Comparative Examples 1-3 was tested, and the test results are shown in the table below:

[0083] Referring to the data in the table above, and based on the comparison between Examples 1-3 and Comparative Examples 1-3, it can be seen that adding 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 them, composite flame retardants have the best effect on improving the flame retardant properties of polyester-cotton fabrics, resulting in excellent flame retardant properties of the prepared polyester-cotton fabrics.

[0084] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0085] The above description is merely an example and illustration of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.

Claims

1. A preparation process for a halogen-free flame-retardant polyester-cotton fabric, characterized in that, Includes the following steps: Step 1: Weigh out 76-82 parts of polyester resin and 4.8-12.2 parts of composite flame retardant according to the following weight proportions; the polyester resin is of type JT-B1. Step 2: Mix polyester resin and composite flame retardant evenly, then melt-extrude through a twin-screw extruder, cool and pelletize, and then melt-spin to obtain flame-retardant polyester fiber; Step 3: Blend flame-retardant polyester fiber and cotton fiber at a mass ratio of 65:35 to obtain polyester-cotton yarn; Step 4: Weave the polyester-cotton yarn into a polyester-cotton fabric to obtain halogen-free flame-retardant polyester-cotton fabric. The composite flame retardant is prepared by the following steps: Step s1: Melamine, terephthalaldehyde, anhydrous sodium acetate and anhydrous ethanol are stirred and reacted. After the reaction is completed, the reaction product is cooled and then evaporated by rotary evaporation to obtain intermediate 1. Step s2: Intermediate 1, 3-aminopropyltriethoxysilane, anhydrous sodium acetate and anhydrous ethanol are stirred and reacted. After the reaction is completed, the reaction product is cooled and then evaporated by rotary evaporation to obtain intermediate 2. Step s3: Intermediate 2, DOPO and anhydrous ethanol are stirred and reacted. After the reaction is completed, the reaction product is cooled, then evaporated by rotary evaporation, then added to ice water, then allowed to stand to precipitate, then vacuum filtered, and the filter cake is dried to obtain organic multi-effect flame retardant. Step s4: Anhydrous magnesium sulfate and deionized water are stirred and reacted. Then activated carbon and sodium dodecylbenzenesulfonate are added and stirred and reacted. Then ammonia water is added dropwise while stirring. After the addition is completed, the reaction is stirred and reacted. After the reaction is completed, the reaction product is cooled, then centrifuged, and the precipitate is washed and dried to obtain inorganic multi-effect flame retardant. Step s5: The organic multi-effect flame retardant, anhydrous ethanol and deionized water are stirred and reacted. Then the pH is adjusted with anhydrous acetic acid and the reaction is continued. Then the inorganic multi-effect flame retardant is added and the reaction is continued. After the reaction is completed, the reaction product is cooled, then centrifuged, and the precipitate is washed and dried to obtain the composite flame retardant.

2. The preparation process of a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that, The 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.

3. The preparation process of a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that, In step s2, the ratio of intermediate 1, 3-aminopropyltriethoxysilane, anhydrous sodium acetate, and anhydrous ethanol 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 ratio of 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 ratio of anhydrous magnesium sulfate, deionized water, activated carbon, sodium dodecylbenzenesulfonate, and ammonia in step s4 is 10-15g: 45-50mL: 3g: 0.2-0.6g: 15-25mL.

6. The preparation process of 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 preparation process of a halogen-free flame-retardant polyester-cotton fabric according to claim 1, characterized in that, The 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.