Processing technology of a fabric for anti-down-feather leakage down jacket

Abstract

The present invention discloses a processing technology for a down-proof and anti-static down jacket fabric, belonging to the technical field of down jacket fabric processing, and is used to solve the technical problems that the down-proof performance, waterproof and breathable performance, and anti-static performance of the existing down jacket fabric need to be further improved; the present invention includes the following steps: using a fabric inner lining film as the inner layer and a base fabric as the outer layer, coating a modified cross-linking agent between the two layers, putting it into a hot melt bonding machine, and performing hot bonding to obtain a down-proof and anti-static down jacket fabric; the present invention prepares the fabric inner lining film with a modified graphene composite, a modified polyurethane, and deionized water, which not only effectively improves the down-proof performance, waterproof and breathable performance of the down jacket fabric, but also improves its anti-static performance and mechanical properties, making it more in line with the requirements of the clothing manufacturing industry for down-proof and anti-static down jacket fabrics.

Description

Technical Field

[0001] The present invention relates to the technical field of fabric processing, and specifically relates to a processing technology for a down-proof down jacket fabric. Background Art

[0002] Down belongs to natural protein fiber and has characteristics such as lightness, thinness, and warmth. It is one of the best natural raw materials for warmth retention. In daily life, down-filled textiles have become popular, especially winter down jackets have become indispensable daily necessities. Down jackets have always been loved by consumers due to their softness, comfort, good warmth retention, and lightness. With the continuous improvement of living standards, the requirements for down jackets have gradually become higher. However, due to various reasons, down jackets will have the problem of down leakage during production and use, which not only seriously affects their overall appearance, but also the leaked down will affect the wearing experience of consumers.

[0003] In the prior art, due to its unique dendritic protein molecular structure, the down in down jackets is prone to friction electrification, resulting in the phenomenon of like charges repelling each other, increasing the risk of down leaking from the micropores or seams of the fabric. To improve the down-proof performance of down jacket fabrics, conductive substances are usually added during the process of making the fabric to improve the conductivity of the fabric, so as to eliminate the influence of static electricity on down leakage of down jackets;

[0004] However, the dispersibility of conductive substances in the fabric substrate and the crosslinking degree with the fabric substrate molecules are poor, resulting in the mechanical strength of conductive fabrics needing to be further improved. Moreover, down jackets are relatively fluffy, and the fabric is prone to friction with the outside world during wearing, resulting in damage to the fabric structure, increasing the risk of down leakage. In addition, conductive materials have poor hydrophobicity, and after being added to the fabric, it affects the waterproof and breathable performance of the fabric, and the processed fabric is difficult to balance the dual performances of down-proof and waterproof and breathable.

[0005] In view of this technical defect, a solution is now proposed. Summary of the Invention

[0006] The purpose of the present invention is to provide a processing technology for a down-proof down jacket fabric, which is used to solve the technical problems that the down jacket fabrics in the prior art need to be further improved in terms of down-proof, waterproof and breathable performance, and mechanical strength.

[0007] The purpose of the present invention can be achieved by the following technical solutions: A processing technology for a down-proof down jacket fabric includes the following steps;

[0008] S1. Under nitrogen protection, isocyanatopropyltriethylsilane, toluene, and 1-aminopyrene are placed in a three-necked flask at a temperature of 50 - 60 °C. After heat preservation reaction for 1 - 2 h, post-treatment is carried out to obtain modified 1-aminopyrene;

[0009] The reaction principle for preparing modified 1-aminopyrene is as follows:

[0010] 1-aminopyrene contains an amino group. In the presence of an isocyanate group, the lone pair of electrons on the nitrogen atom of the amino group can undergo a condensation reaction with the isocyanate group to form modified 1-aminopyrene modified with isocyanatopropyltriethylsilane.

[0011] S2. Place graphene, modified 1-aminopyrene, and ethanol in a three-necked flask heated to 50 - 60 °C, stir for 20 - 30 min, add sodium hydroxide solution to the three-necked flask, keep the temperature for reaction for 90 - 120 min, and perform post-treatment to obtain modified graphene.

[0012] The reaction principle for preparing modified graphene is as follows:

[0013] The siloxane bond in modified 1-aminopyrene hydrolyzes to form silanol, which reacts with the active functional groups on the surface layer of graphene to form a chemical bond, generating modified graphene modified with modified 1-aminopyrene.

[0014] S3. Place N,N-dimethylformamide, modified graphene, and modified iron oxide nanoparticles in a three-necked flask, heat to 100 - 110 °C, ultrasonically disperse for 20 - 30 min, add sodium hydroxide solution to adjust the pH to 8 ± 0.2, keep the temperature for reaction for 0.5 - 1 h, and perform post-treatment to obtain a modified graphene composite.

[0015] The reaction principle for preparing the modified graphene composite is as follows:

[0016] Under weak alkaline conditions, the epoxy group of the modified iron oxide nanoparticles undergoes a ring-opening condensation reaction with the hydroxyl group of the modified graphene to form a covalent bond crosslinking, generating a modified graphene composite modified with modified iron oxide nanoparticles.

[0017] S4. Place the modified graphene composite, modified polyurethane, and N,N-dimethylformamide in a three-necked flask, ultrasonically disperse for 1 - 2 h, and perform electrospinning to obtain a fabric lining film.

[0018] S5. Using the base fabric as the outer layer and the fabric lining film as the inner layer, coat a modified crosslinking agent between the two layers, place it in a hot melt bonding machine, and perform hot bonding to obtain a fabric for anti-feather leakage down jackets.

[0019] Furthermore, in step S1, the dosage ratio of isocyanatopropyltriethylsilane, toluene, and 1-aminopyrene is 1 - 2 g: 250 - 300 mL: 1 - 2 g. The post-treatment step includes: after the reaction is completed, raise the temperature of the three-necked flask to 75 - 85 °C, and distill off toluene under reduced pressure to obtain modified 1-aminopyrene.

[0020] Further, in step S2, the concentration of the sodium hydroxide solution is 0.1 - 0.2 mol / L, and the dosage ratio of graphene, modified 1-aminopyrene, ethanol, and the sodium hydroxide solution is 2 - 3 g: 1 - 5 g: 250 - 300 mL: 30 - 50 mL. The post-treatment steps include: after the reaction is completed, the temperature of the three-necked flask is lowered to room temperature, suction filtration is carried out, the filter cake is washed with purified water until neutral and then dried by suction, the filter cake is transferred to a drying oven at a temperature of 70 - 80 °C, and vacuum dried to constant weight to obtain modified graphene.

[0021] Further, in step S3, the concentration of the sodium hydroxide solution is 3 - 3.5 mol / L, and the dosage ratio of N,N-dimethylformamide, modified graphene, and modified iron oxide nanoparticles is 100 - 150 mL: 1 - 2 g: 1 - 2 g. The post-treatment includes: after the reaction is completed, the temperature of the three-necked flask is lowered to room temperature, suction filtration is carried out, the filter cake is washed with purified water until neutral and then dried by suction, the filter cake is transferred to a drying oven at a temperature of 70 - 80 °C, and vacuum dried to constant weight to obtain a modified graphene composite.

[0022] Further, in step S4, the dosage ratio of the modified graphene composite, modified polyurethane, and N,N-dimethylformamide is 0.5 - 1 g: 2 - 5 g: 50 - 100 mL; in step S5, the base fabric is composed of polyamide fiber and cotton fiber blended in a blending ratio of 20 - 30: 70 - 80, the temperature of the hot pressing process for thermal bonding is 120 - 150 °C, the hot pressing time is 30 - 40 s, and the hot pressing pressure is 1.5 - 2.0 MPa.

[0023] Further, the preparation method of the modified iron oxide nanoparticles is: putting iron oxide nanoparticles, acetone, and KH-560 into a three-necked flask, keeping warm and dispersing for 3 - 4 h, centrifuging, washing the precipitate with acetone for 2 - 3 times, and drying to obtain modified iron oxide nanoparticles.

[0024] The reaction principle for preparing the modified iron oxide nanoparticles is:

[0025] The siloxane groups in KH-560 undergo a condensation reaction with the hydroxyl groups on the surface of the iron oxide nanoparticles to form stable siloxane bonds, obtaining KH-560-modified modified iron oxide nanoparticles.

[0026] Further, the dosage ratio of the iron oxide nanoparticles, acetone, and KH-560 is 2 - 3 g: 50 - 60 mL: 0.5 - 1 g.

[0027] Further, the preparation method of the modified polyurethane includes the following steps:

[0028] A1. Place acetone and dibutyltin dilaurate in a three-necked flask, heat up to 70 - 80 °C, and keep the temperature for reaction for 1 - 2 h to obtain a catalyst solution for standby.

[0029] A2. Place 1-thioglycerol, tridecafluorooctyl methacrylate, acetone, and dimethylphenylphosphine borane in a three-necked flask, heat up to 50 - 60 °C, and stir for 5 - 6 h to obtain a fluorinated monomer.

[0030] The synthesis reaction equation of the fluorinated monomer is:

[0031]

[0032] The synthesis reaction mechanism of the fluorinated monomer is:

[0033] The thiol hydroxyl group in 1-thioglycerol has strong nucleophilicity and can attack the methacrylate double bond in tridecafluorooctyl methacrylate to obtain a fluorinated monomer containing a hydrophobic carbon-fluorine chain.

[0034] The mass spectrometry analysis data of the fluorinated monomer are: 540.03 (100.0%), 541.04 (16.6%), 542.03 (4.5%), 542.04 (2.2%).

[0035] A3. Place isophorone diisocyanate, polyethylene glycol, and acetone in a round-bottom flask, ultrasonically disperse for 30 - 60 min, dropwise add to the catalyst solution, add the fluorinated monomer and 2-hydroxyethyl disulfide, and keep the temperature for reaction for 2 - 3 h to obtain a modified polyurethane.

[0036] Furthermore, in step A1, the dosage ratio of acetone to dibutyltin dilaurate is 20 - 30 mL : 0.1 - 0.5 g; in step A2, the volume ratio of 1-thioglycerol, tridecafluorooctyl methacrylate, acetone, and dimethylphenylphosphine borane is 0.05 - 0.1 : 0.05 - 0.1 : 20 - 30 : 0.05 - 0.1; in step A3, the dosage ratio of isophorone diisocyanate, polyethylene glycol, acetone, catalyst solution, fluorinated monomer, and 2-hydroxyethyl disulfide is 0.1 - 0.5 g : 0.1 - 0.5 g : 50 - 100 mL : 20 - 30 mL : 2 - 5 mL : 0.1 - 0.5 g.

[0037] The synthesis reaction equation of the modified polyurethane is:

[0038]

[0039]

[0040] In the formula: "*" represents the active connection site of the organic chain segment.

[0041] The synthesis reaction mechanism of the modified polyurethane is as follows:

[0042] Isophorone diisocyanate undergoes nucleophilic addition with the alcoholic hydroxyl group of polyethylene glycol under the catalysis of dibutyltin dilaurate to form urethane. A fluorine-containing monomer and 2-hydroxyethyl disulfide are added. The remaining isocyanate in isophorone diisocyanate undergoes nucleophilic addition with the alcoholic hydroxyl groups of the fluorine-containing monomer and 2-hydroxyethyl disulfide respectively, and chain extension is carried out to obtain a modified polyurethane containing dynamic disulfide bonds.

[0043] Furthermore, the preparation method of the modified crosslinking agent includes the following steps: Polypropylene glycol, epichlorohydrin and boron trifluoride ethyl ether are placed in a three-necked flask, heated to 50 - 60 °C, stirred for 2 - 5 h, sodium hydroxide solution is added, and stirring is continued for 2 - 6 h under insulation, and then post-treatment is carried out to obtain the modified crosslinking agent.

[0044] The synthesis reaction equation of the modified crosslinking agent is:

[0045]

[0046] The synthesis reaction principle of the modified crosslinking agent is:

[0047] Boron trifluoride ethyl ether acts as a Lewis acid catalyst. Its electron pair transfers from the oxygen atom to the epoxy group in epichlorohydrin, making the epoxy group positively charged and enhancing its electrophilicity. The alcoholic hydroxyl group of polypropylene glycol is negatively charged and acts as a nucleophile to attack the carbon atom of epichlorohydrin, opening the epoxy group to form an ether bond. Sodium hydroxide solution is added to provide an alkaline environment, the hydroxyl group of chloropropanol is deprotonated to form an alkoxy anion, and the alkoxy anion attacks the chlorinated carbon in the molecule to undergo nucleophilic substitution, and the chloride ion leaves to obtain the modified crosslinking agent.

[0048] Furthermore, the volume ratio of the polypropylene glycol, epichlorohydrin, boron trifluoride ethyl ether and sodium hydroxide solution is 5 - 10:10 - 20:0.3 - 0.5:40 - 60, the concentration of the sodium hydroxide solution is 1.5 - 2 mol / L, and the post-treatment step includes: waiting for the reaction solution to cool to room temperature, extracting it 3 times with an ethyl acetate solution, taking the upper layer solution and carrying out low-pressure rotary evaporation to obtain the modified crosslinking agent, and the ethyl acetate solution is composed of pure water and ethyl acetate according to a volume ratio of 1:1.

[0049] The present invention has the following beneficial effects:

[0050] 1. The anti-down-feather leakage down jacket fabric prepared by the present invention uses a modified graphene composite, modified polyurethane, and deionized water to be ultrasonically dispersed into a spinning solution, and an electrostatic spinning method is used to obtain a fabric lining film. Taking the fabric lining film as the inner layer and the base fabric as the outer layer, a modified crosslinking agent is coated between the two layers, and then put into a hot melt bonding machine for thermal bonding to obtain the anti-down-feather leakage down jacket fabric. The fluorine-containing monomer in the modified polyurethane is synthesized by a thiol-ene click reaction of 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-tridecafluorodecyl methacrylate and 1-thioglycerol catalyzed by dimethylphenylphosphine borane to form a monomer containing a large number of carbon-fluorine bonds. The carbon-fluorine bond has strong hydrophobicity, which increases the hydrophobicity of the anti-down-feather leakage down jacket fabric. The modified polyurethane is composed of hard segments and soft segments and has good flexibility itself, which is conducive to the migration of macromolecular chain segments. Adding 2-hydroxyethyldisulfide to introduce disulfide bonds through chain extension. Under the action of heat and light, the thiol groups can form disulfide bonds again with another thiol group along with the movement of the molecular chain for crosslinking, which can repair the wear of the down jacket fabric during use and improve the anti-down-feather leakage performance of the down jacket fabric.

[0051] 2. The anti-down-feather leakage down jacket fabric prepared by the present invention adds a modified graphene composite composed of modified graphene and modified iron oxide nanoparticles during the electrostatic spinning process. Graphene is a two-dimensional material composed of a single layer of carbon atoms and has good electrical conductivity, which improves the antistatic ability of the anti-down-feather leakage down jacket fabric. Since the static electricity accumulation of the down jacket fabric will cause charges to be generated on the fabric surface and attract the down to move towards the fabric surface, the improvement of the antistatic ability can simultaneously improve the anti-down-feather leakage performance of the down jacket fabric. The modified iron oxide nanoparticles and modified graphene are coated by chemical bonds. Together with 1-aminopyrene and isocyanatopropyltriethoxysilane, they improve the dispersibility of graphene in the electrostatic spinning solution. At the same time, the fluorine-containing branches of the modified polyurethane form hydrophobic forces, strengthening the interaction between the polyurethane and various fillers, enabling the damaged down jacket fabric to not only restore the surface integrity but also repair its electrical conductivity and hydrophobicity, further improving the anti-down-feather leakage property of the down jacket fabric.

[0052] 3. The anti-down-feather leakage down jacket fabric prepared by the present invention coats a modified crosslinking agent between the inner layer and the outer layer during thermal bonding. The modified crosslinking agent uses boron trifluoride diethyl ether as a ring-opening catalyst and sodium hydroxide solution to provide an alkaline environment to promote the synthesis of the modified crosslinking agent. And the modified crosslinking agent undergoes a ring-opening reaction with the hydroxyl groups of the base fabric and the hydroxyl groups in the modified polyurethane to form ether bonds, improving the adhesion between the fabric lining film and the base fabric and increasing the tensile strength of the down jacket fabric. At the same time, the fabric lining film manufactured by the electrostatic spinning technology has a finer diameter and a high specific surface area, which can fill the fiber gaps, reduce the down-feather leakage phenomenon while retaining the breathability of the down jacket fabric. Specific embodiments

[0053] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0054] Embodiment 1

[0055] This embodiment provides a processing technology for a down-proof down jacket fabric, including the following steps:

[0056] S1. Prepare a modified graphene composite

[0057] Weigh: 2 g of iron oxide nanoparticles, 50 mL of acetone, and 0.5 g of KH-560 and place them in a three-necked flask, keep warm and disperse for 3 h, centrifuge, wash the precipitate with acetone three times, and dry to obtain modified iron oxide nanoparticles for standby;

[0058] Weigh: Under nitrogen protection, 250 mL of toluene, 1 g of 1-aminopyrene, and 1 g of isopropyltriethylsilane isocyanate are placed in a three-necked flask at a temperature of 50 °C, keep warm and react for 2 h. After the reaction is completed, the temperature of the three-necked flask is raised to 85 °C, and toluene is removed by reduced pressure distillation to obtain modified 1-aminopyrene;

[0059] Weigh: 2 g of graphene, 1 g of modified 1-aminopyrene, and 250 mL of ethanol are placed in a three-necked flask heated to 55 °C, stir for 30 min, add 30 mL of 0.2 mol / L sodium hydroxide solution to the three-necked flask, keep warm and react for 90 min. After the reaction is completed, the temperature of the three-necked flask is lowered to room temperature, filter by suction, wash the filter cake with purified water until neutral and then drain it, transfer the filter cake to a drying oven at a temperature of 80 °C, and vacuum dry to constant weight to obtain modified graphene;

[0060] Weigh: 100 mL of N,N-dimethylformamide, 1 g of modified graphene, and 1 g of modified iron oxide nanoparticles are placed in a three-necked flask, heated to 100 °C, ultrasonically dispersed for 20 min, add 3 mol / L sodium hydroxide solution to adjust the pH to 8.01, keep warm and react for 1 h. After the reaction is over, the temperature of the three-necked flask is lowered to room temperature, filter by suction, wash the filter cake with purified water until neutral and then drain it, transfer the filter cake to a drying oven at a temperature of 70 °C, and vacuum dry to constant weight to obtain a modified graphene composite.

[0061] S2. Prepare modified polyurethane

[0062] Weigh: 20 mL of acetone and 0.1 g of dibutyltin dilaurate are placed in a three-necked flask, heated to 80 °C, keep warm and react for 2 h to obtain a catalyst solution for standby;

[0063] Weigh: 0.05 mL of 1-thioglycerol, 0.05 mL of tridecafluorooctyl methacrylate, 20 mL of acetone and 0.05 mL of dimethylphenylphosphine borane, place them in a three-necked flask, heat up to 60 °C, stir for 6 h to obtain a fluorinated monomer;

[0064] Weigh: 0.1 g of isophorone diisocyanate, 0.1 g of polyethylene glycol and 50 mL of acetone, place them in a round-bottom flask, ultrasonically disperse for 50 min, dropwise add to 20 mL of a catalyst solution, add 2 mL of the fluorinated monomer and 0.1 g of 2-hydroxyethyl disulfide, keep the temperature for reaction for 2 h to obtain a modified polyurethane.

[0065] S3. Prepare a modified crosslinking agent

[0066] Weigh: Mix 200 mL of ethyl acetate and 200 mL of pure water evenly to obtain an ethyl acetate solution for standby;

[0067] Weigh: Place 5 mL of polypropylene glycol, 10 mL of epichlorohydrin and 0.3 mL of boron trifluoride diethyl etherate in a three-necked flask, heat up to 60 °C, stir for 3 h, add 40 mL of 1.5 mol / L sodium hydroxide solution, keep the temperature and stir for 6 h. After the reaction solution cools to room temperature, extract it 3 times with the ethyl acetate solution, take the upper layer solution and perform low-pressure rotary evaporation to obtain a modified crosslinking agent.

[0068] S4. Prepare a fabric for anti-down leakage down jacket

[0069] Weigh: Place 0.5 g of modified graphene composite, 2 g of modified polyurethane and 50 mL of N,N-dimethylformamide in a three-necked flask, ultrasonically disperse for 2 h to obtain a spinning solution for standby;

[0070] After the spinning solution is left standing to remove air bubbles, it is filled into a 100 mL syringe. A needle with an inner diameter of 0.75 mm and an outer diameter of 1 mm is selected as the spinning needle. Tinfoil is used as the receiving layer and attached to a roller. The voltage of electrospinning is set to 15 kV, the perfusion speed is set to 2 mL / h, the perfusion volume is set to 10 mL, the roller rotation speed is set to 400 r / min, and the distance between the needle and the receiver is 12 cm. After electrospinning, it is dried to obtain a fabric lining film;

[0071] Using TC cloth as the outer layer and the fabric lining film as the inner layer, coat the modified crosslinking agent between the two layers and put it into a hot melt bonding machine to obtain a fabric for anti-down leakage down jacket.

[0072] Example 2

[0073] This example provides a processing technology for a fabric for anti-down leakage down jacket, including the following steps:

[0074] S1. Prepare a modified graphene composite

[0075] Weigh: 2.5 g of iron oxide nanoparticles, 55 mL of acetone and 0.7 g of KH-560 were placed in a three-necked flask, kept warm and dispersed for 3 h, centrifuged, the precipitate was washed 3 times with acetone, and dried to obtain modified iron oxide nanoparticles for standby;

[0076] Weigh: Under nitrogen protection, 270 mL of toluene, 1.5 g of 1-aminopyrene and 1.5 g of isocyanatopropyltriethylsilane were placed in a three-necked flask at 50 °C. After keeping warm and reacting for 2 h, after the reaction was completed, the temperature of the three-necked flask was raised to 85 °C, and toluene was removed by distillation under reduced pressure to obtain modified 1-aminopyrene;

[0077] Weigh: 2.5 g of graphene, 2.5 of modified 1-aminopyrene and 275 mL of ethanol were placed in a three-necked flask heated to 55 °C, stirred for 30 min, 40 mL of 0.2 mol / L sodium hydroxide solution was added to the three-necked flask, and the mixture was kept warm and reacted for 90 min. After the reaction was completed, the temperature of the three-necked flask was lowered to room temperature, filtered by suction, the filter cake was washed with purified water until neutral and then dried by suction, the filter cake was transferred to a drying oven at 80 °C, and vacuum dried to constant weight to obtain modified graphene;

[0078] Weigh: 125 mL of N,N-dimethylformamide, 1.5 g of modified graphene and 1.5 g of modified iron oxide nanoparticles were placed in a three-necked flask, heated to 105 °C, ultrasonically dispersed for 20 min, adjusted to pH = 8.01 with 3.2 mol / L sodium hydroxide solution, and kept warm and reacted for 1 h. After the reaction was completed, the temperature of the three-necked flask was lowered to room temperature, filtered by suction, the filter cake was washed with purified water until neutral and then dried by suction, the filter cake was transferred to a drying oven at 75 °C, and vacuum dried to constant weight to obtain modified graphene composite.

[0079] S2. Preparation of modified polyurethane

[0080] Weigh: 25 mL of acetone and 0.25 g of dibutyltin dilaurate were placed in a three-necked flask, heated to 80 °C, and kept warm and reacted for 2 h to obtain a catalyst solution for standby;

[0081] Weigh: 0.07 mL of 1-thioglycerol, 0.07 mL of tridecafluorooctyl methacrylate, 25 mL of acetone and 0.06 mL of dimethylphenylphosphine borane were placed in a three-necked flask, heated to 60 °C, and stirred for 6 h to obtain a fluorine-containing monomer;

[0082] Weigh: 0.25 g of isophorone diisocyanate, 0.25 g of polyethylene glycol and 75 mL of acetone were placed in a round-bottomed flask, ultrasonically dispersed for 50 min, dropped into 25 mL of the catalyst solution, added 4.5 mL of the fluorine-containing monomer and 0.25 g of 2-hydroxyethyl disulfide, and kept warm and reacted for 2 h to obtain modified polyurethane.

[0083] S3. Preparation of modified crosslinking agent

[0084] Weigh: Mix 250 mL of ethyl acetate and 250 mL of pure water evenly to obtain an ethyl acetate solution for standby;

[0085] Weigh: Place 7.5 mL of polypropylene glycol, 15 mL of epichlorohydrin, and 0.4 mL of boron trifluoride diethyl etherate in a three-necked flask, heat up to 60 °C, stir for 3 h, add 40 mL of 50 mL 1.5 mol / L sodium hydroxide solution, keep warm and stir for 6 h. After the reaction solution cools to room temperature, extract it 3 times with the ethyl acetate solution, take the upper layer solution and perform low-pressure rotary evaporation to obtain a modified crosslinking agent.

[0086] S4. Prepare the anti-down leakage down jacket fabric

[0087] Weigh: Place 0.75 g of modified graphene composite, 3.5 g of modified polyurethane, and 75 mL of N,N-dimethylformamide in a three-necked flask, and perform ultrasonic dispersion for 2 h to obtain a spinning solution for standby;

[0088] After the spinning solution is left standing to remove air bubbles, it is filled into a 100 mL syringe. A needle with an inner diameter of 0.75 mm and an outer diameter of 1 mm is selected as the spinning needle. Tin foil is used as the receiving layer and attached to the roller. The voltage of electrospinning is set to 15 kV, the perfusion speed is set to 2 mL / h, the perfusion volume is set to 10 mL, the roller rotation speed is set to 400 r / min, and the distance between the needle and the receiver is 12 cm. After electrospinning, dry it to obtain a fabric lining film;

[0089] Using TC cloth as the outer layer and the fabric lining film as the inner layer, coat the modified crosslinking agent between the two layers and put it into a hot melt bonding machine to obtain the anti-down leakage down jacket fabric.

[0090] Example 3

[0091] This example provides a processing technology for an anti-down leakage down jacket fabric, including the following steps:

[0092] S1. Prepare the modified graphene composite

[0093] Weigh: Place 3 g of iron oxide nanoparticles, 60 mL of acetone, and 1.5 g of KH-560 in a three-necked flask, keep warm and disperse for 3 h, centrifuge, wash the precipitate with acetone 3 times, and dry it to obtain modified iron oxide nanoparticles for standby;

[0094] Weigh: Under nitrogen protection, place 300 mL of toluene, 2 g of 1-aminopyrene, and 2 g of isocyanatopropyltriethylsilane in a three-necked flask at a temperature of 50 °C, keep warm and react for 2 h. After the reaction is completed, raise the temperature of the three-necked flask to 85 °C and distill off toluene under reduced pressure to obtain modified 1-aminopyrene;

[0095] Weigh: 3 g of graphene, 5 g of modified 1-aminopyrene, and 300 mL of ethanol and place them in a three-necked flask heated to 40 °C. Stir for 30 min. Add 50 mL of 0.2 mol / L sodium hydroxide solution to the three-necked flask, and keep the temperature for reaction for 90 min. After the reaction is completed, lower the temperature of the three-necked flask to room temperature, perform suction filtration, wash the filter cake with purified water until it is neutral, and then dry it by suction. Transfer the filter cake to a drying oven at 80 °C and vacuum dry it to constant weight to obtain modified graphene;

[0096] Weigh: 150 mL of N,N-dimethylformamide, 2 g of modified graphene, and 2 g of modified iron oxide nanoparticles and place them in a three-necked flask. Heat to 110 °C and ultrasonically disperse for 20 min. Add 3.5 mol / L sodium hydroxide solution to adjust the pH to 8.02, and keep the temperature for reaction for 1 h. After the reaction is completed, lower the temperature of the three-necked flask to room temperature, perform suction filtration, wash the filter cake with purified water until it is neutral, and then dry it by suction. Transfer the filter cake to a drying oven at 80 °C and vacuum dry it to constant weight to obtain a modified graphene composite.

[0097] S2. Preparation of modified polyurethane

[0098] Weigh: 30 mL of acetone and 0.5 g of dibutyltin dilaurate and place them in a three-necked flask. Heat to 80 °C and keep the temperature for reaction for 2 h to obtain a catalyst solution for standby;

[0099] Weigh: 0.1 mL of 1-thioglycerol, 0.1 mL of tridecafluorooctyl methacrylate, 30 mL of acetone, and 0.1 mL of dimethylphenylphosphine borane and place them in a three-necked flask. Heat to 60 °C and stir for 6 h to obtain a fluorinated monomer;

[0100] Weigh: 0.5 g of isophorone diisocyanate, 0.5 g of polyethylene glycol, and 100 mL of acetone and place them in a round-bottomed flask. Ultrasonically disperse for 50 min, dropwise add it to 30 mL of the catalyst solution, add 5 mL of the fluorinated monomer and 0.5 g of 2-hydroxyethyl disulfide, and keep the temperature for reaction for 2 h to obtain modified polyurethane.

[0101] S3. Preparation of modified crosslinking agent

[0102] Weigh: Mix 300 mL of ethyl acetate and 300 mL of pure water evenly to obtain an ethyl acetate solution for standby;

[0103] Weigh: Place 10 mL of polypropylene glycol, 20 mL of epichlorohydrin, and 0.5 mL of boron trifluoride diethyl etherate in a three-necked flask. Heat to 60 °C and stir for 3 h. Add 60 mL of 2 moL / L sodium hydroxide solution, keep the temperature and stir for 6 h. After the reaction solution cools to room temperature, extract it 3 times with the ethyl acetate solution, take the upper layer solution and perform low-pressure rotary evaporation to obtain a modified crosslinking agent.

[0104] S4. Preparation of anti-down leakage down jacket fabric

[0105] Weigh: 1 g of modified graphene composite, 5 g of modified polyurethane and 100 mL of N,N-dimethylformamide and place them in a three-necked flask. Ultrasonically disperse for 2 h to obtain a spinning solution for standby;

[0106] After the spinning solution is left standing to remove air bubbles, it is loaded into a 100 mL syringe. A needle with an inner diameter of 0.75 mm and an outer diameter of 1 mm is selected as the spinning needle. Tin foil is used as the receiving layer and attached to the roller. The voltage of electrospinning is set at 15 kV, the perfusion speed is set at 2 mL / h, the perfusion volume is set at 10 mL, the roller rotation speed is set at 400 r / min, and the distance between the needle and the receiver is 12 cm. After electrospinning, it is dried to obtain a fabric lining film;

[0107] Using TC cloth as the outer layer and the fabric lining film as the inner layer, a modified crosslinking agent is coated between the two layers to obtain a down-proof down jacket fabric.

[0108] Comparative Example 1

[0109] The difference between this comparative example and Example 3 is that the step of modified iron oxide nanoparticles in step S1 is cancelled, and silica nanoparticles are used to replace the modified iron oxide nanoparticles in equal amount during the preparation of the modified graphene composite.

[0110] Comparative Example 2

[0111] The difference between this comparative example and Example 3 is that the step of preparing the fluorinated monomer in step S2 is cancelled, and 1-thioglycerol is used to replace the fluorinated monomer in equal amount during the preparation of the modified polyurethane.

[0112] Comparative Example 3

[0113] The difference between this comparative example and Example 3 is that the use of the modified crosslinking agent when preparing the spinning solution in step S4 is cancelled, and the modified crosslinking agent is not coated between the inner and outer layers during thermal bonding.

[0114] Performance test:

[0115] Refer to the standard GB / T 3923.2-2013 "Textiles - Tensile properties of fabrics - Part 2: Determination of breaking force (grab method)" to test the breaking force of the down-proof down jacket fabrics prepared in Examples 1-3 and Comparative Examples 1-3;

[0116] Refer to the standard GB / T 4744-2013 "Textiles - Detection and evaluation of waterproof properties - Hydrostatic pressure method" to test the waterproof property of the down-proof down jacket fabrics prepared in Examples 1-3 and Comparative Examples 1-3;

[0117] The air permeability of the anti-down-feather leakage down jacket fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was tested with reference to the standard GB / T 5453-1997 "Textiles - Determination of air permeability of fabrics".

[0118] The antistatic property of the anti-down-feather leakage down jacket fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was tested with reference to the standard GB / T 12703.4-2010 "Textiles - Evaluation of electrostatic properties - Part 4: Resistivity".

[0119] With reference to the standard GB / T 12705.1-2024 "Textiles - Test method for anti-down-feather leakage - Part 1: Friction method", the anti-down-feather leakage property of the anti-down-feather leakage down jacket fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was tested. The specific data are shown in Table 1.

[0120] Table 1. Performance test data of the specimens

[0121] Project Group Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Breaking Strength / N 200 211 205 175 180 156 Hydrostatic Pressure Resistance Level / grade 4 5 4 2 3 4 <![CDATA[Air permeability / mm·s -1 > 0.451 0.532 0.482 0.449 0.423 0.411 Resistivity / Ω·cm 0.582 0.535 0.586 0.710 0.540 0.619 Number of Feather Leakage / root 7 4 8 20 12 22

[0122] Data analysis:

[0123] By comparing and analyzing the data of Examples 1-3 and Comparative Examples 1-3, the breaking strength of the anti-down-feather leakage down jacket fabric prepared in the present invention reached 211 N, the hydrostatic pressure resistance level reached 5, the air permeability was 0.532 mm·s -1 , the resistivity was 0.535 Ω·cm and the number of down-feather leakage roots was 4, indicating that the anti-down-feather leakage down jacket fabric prepared in the present invention has good anti-down-feather leakage performance, waterproof and air permeability, mechanical properties and antistatic properties;

[0124] The flame retardant property of Comparative Example 1 was basically the same as the air permeability of Examples 1-3. Its breaking strength, hydrostatic pressure resistance level and resistivity decreased, and the number of down-feather leakage roots increased, indicating that adding modified iron oxide nanoparticles in the process of preparing the modified graphene composite can improve the dispersibility of the modified graphene composite in the spinning solution, and further improve the anti-down-feather leakage performance, waterproof performance, mechanical properties and antistatic properties of the anti-down-feather leakage down jacket fabric;

[0125] The breaking strength and hydrostatic pressure resistance level of Comparative Example 2 decreased, and the number of down-feather leakage roots increased, showing a decrease compared with Examples 1-3, indicating that the modified polyurethane prepared with fluorine-containing monomers can improve the waterproof performance, mechanical properties and anti-down-feather leakage performance of the anti-down-feather leakage down jacket fabric;

[0126] The breaking strength, hydrostatic pressure resistance level and resistivity of Comparative Example 3 decreased, and the number of down-feather leakage roots increased, indicating that the modified crosslinking agent can improve the anti-down-feather leakage performance, waterproof and air permeability, mechanical properties and antistatic properties of the anti-down-feather leakage down jacket fabric;

[0127] The above content is only an example and illustration of the structure of the present invention. Those skilled in the art to which the present technology pertains can make various modifications or supplements to the described specific embodiments or use similar methods for substitution, as long as they do not deviate from the structure of the invention or exceed the scope defined by this claims, they shall fall within the protection scope of the present invention.

Claims

1. A processing technology for a down-proof down jacket fabric, characterized in that, It includes the following steps; S1. Under nitrogen protection, isocyanatopropyltriethylsilane, toluene and 1-aminopyrene are placed in a three-necked flask at a temperature of 50 - 60 °C. After heat preservation reaction for 1 - 2 h, post-treatment is carried out to obtain modified 1-aminopyrene; S2. Graphene, modified 1-aminopyrene and ethanol are placed in a three-necked flask heated to 50 - 60 °C, stirred for 20 - 30 min, sodium hydroxide solution is added to the three-necked flask, heat preservation reaction is carried out for 90 - 120 min, and post-treatment is carried out to obtain modified graphene; S3. N,N-dimethylformamide, modified graphene and modified iron oxide nanoparticles are placed in a three-necked flask, heated to 100 - 110 °C, ultrasonically dispersed for 20 - 30 min, sodium hydroxide solution is added to adjust the pH to 8 ± 0.2, heat preservation reaction is carried out for 0.5 - 1 h, and post-treatment is carried out to obtain modified graphene composite; S4. The modified graphene composite, fluorine-containing monomer modified polyurethane and N,N-dimethylformamide are placed in a three-necked flask, ultrasonically dispersed for 1 - 2 h, and electrospun to obtain a fabric lining membrane; S5. Using the base fabric as the outer layer and the fabric lining membrane as the inner layer, a modified cross-linking agent is coated between the two layers, and then put into a hot melt bonding machine for hot bonding to obtain an anti-feather leakage down jacket fabric.

2. The processing technology of a down-proof down jacket fabric according to claim 1, characterized in that, In step S1, the dosage ratio of isocyanatopropyltriethylsilane, toluene and 1-aminopyrene is 1 - 2 g: 250 - 300 mL: 1 - 2 g; in step S2, the concentration of the sodium hydroxide solution is 0.1 - 0.2 mol / L, and the dosage ratio of graphene, modified 1-aminopyrene, ethanol and sodium hydroxide solution is 2 - 3 g: 1 - 5 g: 250 - 300 mL: 30 - 50 mL; in step S3, the concentration of the sodium hydroxide solution is 3 - 3.5 mol / L, and the dosage ratio of N,N-dimethylformamide, modified graphene and modified iron oxide nanoparticles is 100 - 150 mL: 1 - 2 g: 1 - 2 g; in step S4, the dosage ratio of the modified graphene composite, fluorine-containing monomer modified polyurethane and N,N-dimethylformamide is 0.5 - 1 g: 2 - 5 g: 50 - 100 mL; in step S5, the base fabric is composed of nylon fiber and cotton fiber blended at a blending ratio of 20 - 30: 70 - 80, the temperature of the hot pressing process for hot bonding is 120 - 150 °C, the hot pressing time is 30 - 40 s, and the hot pressing pressure is 1.5 - 2.0 MPa.

3. The processing technology of a down-proof down jacket fabric according to claim 1, characterized in that, The preparation method of the modified iron oxide nanoparticles is as follows: Iron oxide nanoparticles, acetone and KH-560 are placed in a three-necked flask, heat preservation dispersion is carried out for 3 - 4 h, centrifuged, the precipitate is washed with acetone for 2 - 3 times, and dried to obtain modified iron oxide nanoparticles.

4. The processing technology of a down-proof down jacket fabric according to claim 3, characterized in that, The dosage ratio of the modified iron oxide nanoparticles, acetone and KH-560 is 2 - 3 g: 50 - 60 mL: 0.5 - 1 g.

5. The processing technology of a down-proof down jacket fabric according to claim 1, characterized in that, The preparation method of the fluorine-containing monomer modified polyurethane includes the following steps: A1. Acetone and dibutyltin dilaurate are placed in a three-necked flask, heated to 70 - 80 °C, and heat preservation reaction is carried out for 1 - 2 h to obtain a catalyst solution for standby; A2. Place 1-thioglycerol, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-tridecafluorodecyl methacrylate, acetone, and dimethylphenylphosphine borane in a three-necked flask, heat up to 50 - 60 °C, and stir for 5 - 6 h to obtain a fluorine-containing monomer. A3. Place isophorone diisocyanate, polyethylene glycol, and acetone in a round-bottom flask, ultrasonically disperse for 30 - 60 min, dropwise add to the catalyst solution, add the fluorine-containing monomer and 2-hydroxyethyl disulfide, and carry out a heat preservation reaction for 2 - 3 h to obtain a fluorine-containing monomer-modified polyurethane.

6. The processing technology of a down-proof down jacket fabric according to claim 5, characterized in that, In step A1, the dosage ratio of the acetone to dibutyltin dilaurate is 20 - 30 mL:0.1 - 0.5 g; in step A2, the volume ratio of 1-thioglycerol, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-tridecafluorodecyl methacrylate, acetone, and dimethylphenylphosphine borane is 0.05 - 0.1:0.05 - 0.1:20 - 30:0.05 - 0.1; in step A3, the dosage ratio of isophorone diisocyanate, polyethylene glycol, acetone, catalyst solution, fluorine-containing monomer, and 2-hydroxyethyl disulfide is 0.1 - 0.5 g:0.1 - 0.5 g:50 - 100 mL:20 - 30 mL:2 - 5 mL:0.1 - 0.5 g.

7. The processing technology of a down-proof down jacket fabric according to claim 1, characterized in that, The preparation method of the modified cross-linking agent comprises the following steps: Place polypropylene glycol, epichlorohydrin, and boron trifluoride diethyl etherate in a three-necked flask, heat up to 50 - 60 °C, stir for 2 - 5 h, add sodium hydroxide solution, carry out a heat preservation stirring for 2 - 6 h, and perform post-treatment to obtain the modified cross-linking agent.

8. The processing technology of a down-proof down jacket fabric according to claim 7, characterized in that, The volume ratio of the polypropylene glycol, epichlorohydrin, boron trifluoride diethyl etherate, and sodium hydroxide solution is 5 - 10:10 - 20:0.3 - 0.5:40 - 60 mL, and the concentration of the sodium hydroxide solution is 1.5 - 2 mol / L.

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