Preparation method of anti-mosquito fabric

By applying flame retardant reagent and mosquito-repellent microcapsules on the base material, combined with phosphorus-containing quaternary ammonium salt treatment, the problem of mosquito infestation during camping in the wild is solved, and the flame retardant and mosquito-repellent functions of the fabric are realized.

CN119980716APending Publication Date: 2025-05-13ZHEJIANG DONGJIN NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202311492053.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-11-10
Publication Date
2025-05-13

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Abstract

The invention discloses a preparation method of an anti-mosquito fabric. The preparation method comprises a step of treating a base material fabric with phosphorus-containing quaternary ammonium salt organosiloxane and a step of coating the base material fabric with an anti-mosquito microcapsule coating. The step of treating the base material fabric by using the phosphorus-containing quaternary ammonium salt organosiloxane specifically comprises the following steps: preparing an 8wt% phosphorus-containing quaternary ammonium salt organosiloxane ethanol / water mixed solution (the volume ratio of ethanol to water is 60: 40), adjusting the pH value to 5-5.5, putting the base material fabric into the solution, carrying out a dipping reaction for 30 minutes, then taking out the base material fabric, and drying the base material fabric. The step of coating the base material fabric with the anti-mosquito microcapsule coating specifically comprises the following steps: blending a waterborne polyurethane emulsion, an anti-mosquito microcapsule emulsion, a cross-linking agent and a thickening agent into coating slurry, then coating the surface of the base material fabric with the coating slurry, drying at the temperature of 120 DEG C for 60 seconds, and baking at the temperature of 150 DEG C for 60 seconds. The fabric prepared by the method has good anti-mosquito and flame-retardant functions.
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Description

Technical Field

[0001] The invention relates to a method for preparing mosquito-proof fabric, and belongs to the field of functional textile fabrics. Background Art

[0002] Camping is a popular leisure activity in recent years, which has brought about the consumption of camping tent fabrics. In the wild, mosquitoes are a headache. Mosquito bites not only cause skin itching, but also spread diseases and cause harm to health.

[0003] In a tent, it is obviously inappropriate to use special sound waves or light waves to lure or repel mosquitoes, or to use natural enemies or microorganisms to kill or repel mosquitoes; killing mosquitoes with mosquito coils or insecticide sprays can easily cause human health problems. Summary of the invention

[0004] The present invention aims to provide a method for preparing a mosquito-proof fabric, and a flame retardant agent and mosquito-proof microcapsules are applied on the surface of a base fabric to prepare a fabric with flame retardant and mosquito-proof functions.

[0005] To achieve the above objectives, the present invention adopts the following technical solutions.

[0006] A method for preparing mosquito-proof fabric, comprising the steps of treating a substrate fabric with a phosphorus-containing quaternary ammonium salt organic siloxane and coating the substrate fabric with a mosquito-proof microcapsule coating;

[0007] The anti-mosquito microcapsule coating is composed of 30 parts of aqueous polyurethane emulsion, 7 parts of anti-mosquito microcapsule emulsion, 3 parts of cross-linking agent and 2 parts of thickener in parts by mass;

[0008] The phosphorus-containing quaternary ammonium salt organosiloxane is prepared by:

[0009] 17.3 g of diethyl chlorophosphate and 50 mL of tetrahydrofuran were added to the S1 reactor, and nitrogen was introduced at the same time. 9 g of N, N-dimethylethanolamine and 3 g of triethylamine were added and stirred in an ice-water bath for 4 h. After the reaction was complete, the organic solvent tetrahydrofuran was removed by vacuum distillation, and the mixture was filtered to obtain (triethyl phosphate) N, N-dimethylamine;

[0010] S2: In a reactor equipped with a stirrer, a condenser and a thermometer, add 22.5 g of (triethyl phosphate) N,N-dimethylamine, 24 g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane and 140 g of isopropanol, stir and mix evenly, reflux at 70°C until the reactant becomes transparent, and then react for 2 hours. Then, remove the isopropanol at 0.01 MPa to obtain a viscous liquid, which is a phosphorus-containing quaternary ammonium salt organosiloxane.

[0011] The step of treating the substrate fabric with the phosphorus-containing quaternary ammonium salt organosiloxane specifically comprises preparing an 8wt% phosphorus-containing quaternary ammonium salt organosiloxane ethanol / water mixed solution (ethanol / water volume ratio 60:40), adjusting the pH to 5-5.5, immersing the substrate fabric in the solution for reaction for 30 minutes, and then taking out the substrate fabric and drying it.

[0012] The step of coating the anti-mosquito microcapsule coating on the substrate fabric specifically comprises mixing water-based polyurethane emulsion, anti-mosquito microcapsule emulsion, crosslinking agent and thickener into coating slurry, then coating the coating slurry on the surface of the substrate fabric, drying and baking.

[0013] The anti-mosquito microcapsule emulsion is prepared by polymerization of hydroxyethyl acrylate, acrylic resin, KH-570, mosquito repellent, initiator, emulsifier and water.

[0014] The mosquito repellent is a mixture of citronella oil and catnip oil.

[0015] The emulsifier is a mixture of sodium dodecylbenzene sulfonate, OP-10 and polyvinyl alcohol.

[0016] The anti-mosquito microcapsule emulsion is prepared by:

[0017] a. Mix hydroxyethyl acrylate and acrylic resin evenly, then add mosquito repellent and KH-570 and mix well;

[0018] b. Add emulsifier and initiator into water and stir to dissolve;

[0019] c. Add the mixture of step a to the water of step b, stir and emulsify to form an emulsion;

[0020] d. At room temperature, irradiate the emulsion of step c with 450-500nm blue light to make the emulsion undergo polymerization reaction to obtain mosquito repellent microcapsule emulsion.

[0021] The invention discloses a method for preparing a mosquito-proof fabric, comprising the steps of treating a substrate fabric with a phosphorus-containing quaternary ammonium salt organosiloxane and coating a mosquito-proof microcapsule coating on the substrate fabric. The silaneoxy groups in the phosphorus-containing quaternary ammonium salt organosiloxane react with the groups on the substrate fabric and are grafted on the surface of the fabric, so that the fabric has flame retardant properties and meets the flame retardant requirements of outdoor fabrics. The quaternary ammonium cations contained in the phosphorus-containing quaternary ammonium salt organosiloxane combine with the anions of the mosquito-proof microcapsule coating, and the condensation of the silaneoxy groups enhances the bonding force between the coating and the fabric. The mosquito-repellent substance is coated in the microcapsule and is slowly released during the use of the mosquito-proof fabric, thereby achieving a long-lasting mosquito-repellent effect. The fabric prepared by the method of the invention has good mosquito-proof and flame-retardant functions. DETAILED DESCRIPTION

[0022] The technical solution of the present invention is described in detail below through specific embodiments.

[0023] The "part" referred to in the present invention is a unit of weight.

[0024] The invention discloses a method for preparing mosquito-proof fabric, comprising the steps of treating a substrate fabric with phosphorus-containing quaternary ammonium salt organic siloxane and coating the substrate fabric with a mosquito-proof microcapsule coating.

[0025] The step of treating the substrate fabric with the phosphorus-containing quaternary ammonium salt organosiloxane specifically comprises preparing an 8wt% phosphorus-containing quaternary ammonium salt organosiloxane ethanol / water mixed solution (ethanol / water volume ratio 60:40), adjusting the pH to 5-5.5, immersing the substrate fabric in the solution for reaction for 30 minutes, and then taking out the substrate fabric and drying it.

[0026] The step of coating the anti-mosquito microcapsule coating on the substrate fabric specifically comprises mixing the aqueous polyurethane emulsion, the anti-mosquito microcapsule emulsion, the crosslinking agent and the thickener into a coating slurry, and then coating the coating slurry on the surface of the substrate fabric, drying (120°C, 60s), and baking (150°C, 60s). The anti-mosquito microcapsule coating is composed of 30 parts of aqueous polyurethane emulsion, 7 parts of anti-mosquito microcapsule emulsion, 3 parts of crosslinking agent and 2 parts of thickener in parts by mass.

[0027] The phosphorus-containing quaternary ammonium salt organosiloxane is prepared by:

[0028] 17.3 g of diethyl chlorophosphate and 50 mL of tetrahydrofuran were added to the S1 reactor, and nitrogen was introduced at the same time. 9 g of N, N-dimethylethanolamine and 3 g of triethylamine were added and stirred in an ice-water bath for 4 h. After the reaction was complete, the organic solvent tetrahydrofuran was removed by vacuum distillation, and the mixture was filtered to obtain (triethyl phosphate) N, N-dimethylamine;

[0029] S2: In a reactor equipped with a stirrer, a condenser and a thermometer, add 22.5 g of (triethyl phosphate) N,N-dimethylamine, 24 g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane and 140 g of isopropanol, stir and mix evenly, reflux at 70°C until the reactant becomes transparent, and then react for 2 hours. Then, remove the isopropanol at 0.01 MPa to obtain a viscous liquid, which is a phosphorus-containing quaternary ammonium salt organosiloxane.

[0030] The reaction formula for preparing phosphorus-containing quaternary ammonium salt organosiloxane is as follows:

[0031]

[0032] The anti-mosquito microcapsule emulsion is prepared by polymerization of 15 parts of hydroxyethyl acrylate, 50 parts of acrylic resin, 6 parts of KH-570 (γ-methacryloxypropyltrimethoxysilane), 14 parts of mosquito repellent, 0.9 parts of initiator, 6 parts of emulsifier and 400 parts of water.

[0033] The mosquito repellent is a mixture of citronella oil and catnip oil, wherein the mass ratio of the citronella oil to the catnip oil is 1:1.

[0034] The emulsifier is a mixture of sodium dodecylbenzene sulfonate, OP-10 and polyvinyl alcohol, wherein the mass ratio of sodium dodecylbenzene sulfonate, OP-10 and polyvinyl alcohol is 3:2:1.

[0035] The initiator is a camphorquinone / tertiary amine composition with a mass ratio of 1:1.

[0036] The anti-mosquito microcapsule emulsion is prepared by:

[0037] a. Mix hydroxyethyl acrylate and acrylic resin evenly, then add mosquito repellent and KH-570 and mix well;

[0038] b. Add emulsifier and initiator into water and stir to dissolve;

[0039] c. Add the mixture of step a to the water of step b, stir and emulsify to form an emulsion;

[0040] d. At room temperature, irradiate the emulsion of step c with 450-500nm blue light to make the emulsion undergo polymerization reaction to obtain mosquito repellent microcapsule emulsion.

[0041] The mosquito repellent or mosquito repellent microcapsules are adhered to the surface of the fabric by an adhesive to form a durable and stable mosquito-proof fabric.

[0042] Before applying flame retardant and mosquito-proof coating, the base fabric needs to undergo conventional scouring pre-treatment to remove surface oil stains. After the pre-treatment of decontamination and impurity removal, appropriate alkali reduction can also be carried out.

[0043] Scouring pretreatment of substrate fabric: put the substrate fabric into the pretreatment liquid → heat to 130℃ and keep warm for 30min → cool down and wash with water; the pretreatment liquid contains 5g / L NaOH, 3g / L scouring agent, 3g / L chelating dispersant, and the rest is water, with a bath ratio of 1:8.

[0044] Alkali reduction process for base fabric: NaOH 8g / L, bath ratio 1:8, temperature 100℃ for 45min, then acid neutralization, water washing and drying.

[0045] The scouring agent, chelating dispersant and the like involved in the scouring pre-treatment step are all commercially available conventional products.

[0046] Embodiment 1:

[0047] Base material: grey cloth, warp and weft: 150D×150D, composition: 100% polyester.

[0048] Refining pretreatment of base fabric grey cloth: the base fabric is put into the pretreatment liquid → heated to 130℃ and kept warm for 30min → cooled and washed; the pretreatment liquid contains 5g / L NaOH, 3g / L scouring agent, 3g / L chelating dispersant, and the rest is water.

[0049] Phosphorus-containing quaternary ammonium salt organosiloxane treated substrate fabrics:

[0050] Ethanol / water are mixed in a volume ratio of 60:40, and then phosphorus-containing quaternary ammonium salt organosiloxane is added to prepare an 8wt% solution, the pH is adjusted to 5-5.5, the substrate fabric is immersed in the solution for reaction for 30 minutes, and then the substrate fabric is taken out and dried at 100°C for 60 seconds to make a flame retardant fabric.

[0051] Flame retardant performance: afterflaming time 0s, smoldering time 0s, damage length 73mm. The flame retardant performance test of fabrics refers to "GB / T5455-2014 Textile Combustion Performance - Determination of Damage Length, Smoldering and Afterflaming Time in Vertical Direction".

[0052] Embodiment 2:

[0053] Base material: grey cloth, warp and weft: 150D×150D, composition: 100% polyester.

[0054] Refining pretreatment of base fabric grey cloth: the base fabric is put into the pretreatment liquid → heated to 130℃ and kept warm for 30min → cooled and washed; the pretreatment liquid contains 5g / L NaOH, 3g / L scouring agent, 3g / L chelating dispersant, and the rest is water.

[0055] A method for preparing mosquito-proof fabrics, comprising the steps of treating a substrate fabric with a phosphorus-containing quaternary ammonium salt organic siloxane and coating the substrate fabric with a mosquito-proof microcapsule coating. Specifically:

[0056] (1) preparing an 8 wt % ethanol / water mixed solution of phosphorus-containing quaternary ammonium salt organosiloxane (ethanol / water volume ratio 60:40), adjusting the pH to 5-5.5, immersing the substrate fabric in the solution for 30 min, then taking out the substrate fabric and drying it;

[0057] (2) 30 parts of water-based polyurethane emulsion, 7 parts of mosquito-proof microcapsule emulsion, 3 parts of cross-linking agent, and 2 parts of thickener are prepared into a coating slurry, and then the coating slurry is applied to the surface of the substrate fabric, dried (120° C., 60 seconds), and baked (150° C., 60 seconds) to form a mosquito-proof microcapsule coating, thereby obtaining the mosquito-proof fabric.

[0058] The relevant properties of the mosquito-proof fabric prepared by the embodiment method were tested according to the method of GB / T 30126-2013 "Testing and Evaluation of Mosquito-proof Properties of Textiles". The results are shown in Tables 1 and 2 below.

[0059] Table 1 Durability of mosquito repellent effect of mosquito repellent fabrics

[0060]

[0061] Table 2 Washing resistance of mosquito repellent fabrics

[0062]

Claims

1. A method for preparing a mosquito-proof fabric, comprising the steps of treating a substrate fabric with a phosphorus-containing quaternary ammonium salt organosiloxane and coating the substrate fabric with a mosquito-proof microcapsule coating; the mosquito-proof microcapsule coating, in parts by mass, is composed of 30 parts of an aqueous polyurethane emulsion, 7 parts of a mosquito-proof microcapsule emulsion, 3 parts of a cross-linking agent, and 2 parts of a thickener; The phosphorus-containing quaternary ammonium salt organosiloxane is prepared by: 17.3 g of diethyl chlorophosphate and 50 mL of tetrahydrofuran were added to the S1 reactor, and nitrogen was introduced at the same time. 9 g of N, N-dimethylethanolamine and 3 g of triethylamine were added and stirred in an ice-water bath for 4 h. After the reaction was complete, the organic solvent tetrahydrofuran was removed by vacuum distillation, and the mixture was filtered to obtain (triethyl phosphate) N, N-dimethylamine; S2: In a reactor equipped with a stirrer, a condenser and a thermometer, add 22.5 g of (triethyl phosphate) N,N-dimethylamine, 24 g of γ-(2,3-epoxypropoxy)propyltrimethoxysilane and 140 g of isopropanol, stir and mix evenly, reflux at 70°C until the reactant becomes transparent, and then react for 2 hours. Then, remove the isopropanol at 0.01 MPa to obtain a viscous liquid, which is a phosphorus-containing quaternary ammonium salt organosiloxane.

2. The method for preparing the mosquito-proof fabric according to claim 1, characterized in that: The step of treating the substrate fabric with the phosphorus-containing quaternary ammonium salt organosiloxane specifically comprises preparing an 8wt% phosphorus-containing quaternary ammonium salt organosiloxane ethanol / water mixed solution (ethanol / water volume ratio 60:40), adjusting the pH to 5-5.5, immersing the substrate fabric in the solution for reaction for 30 minutes, and then taking out the substrate fabric and drying it.

3. The method for preparing the mosquito-proof fabric according to claim 1, characterized in that: The step of coating the anti-mosquito microcapsule coating on the substrate fabric specifically comprises mixing water-based polyurethane emulsion, anti-mosquito microcapsule emulsion, crosslinking agent and thickener into coating slurry, then coating the coating slurry on the surface of the substrate fabric, drying and baking.

4. The method for preparing the mosquito-proof fabric according to claim 1, characterized in that: The anti-mosquito microcapsule emulsion is prepared by polymerization of hydroxyethyl acrylate, acrylic resin, KH-570, mosquito repellent, initiator, emulsifier and water.

5. The method for preparing the mosquito-proof fabric according to claim 4, characterized in that: The mosquito repellent is a mixture of citronella oil and catnip oil.

6. The method for preparing the mosquito-proof fabric according to claim 4, characterized in that: The emulsifier is a mixture of sodium dodecylbenzene sulfonate, OP-10 and polyvinyl alcohol.

7. The method for preparing the mosquito-proof fabric according to claim 1 or 4, characterized in that: The anti-mosquito microcapsule emulsion is prepared by: a. Mix hydroxyethyl acrylate and acrylic resin evenly, then add mosquito repellent and KH-570 and mix well; b. Add emulsifier and initiator into water and stir to dissolve; c. Add the mixture of step a to the water of step b, stir and emulsify to form an emulsion; d. At room temperature, irradiate the emulsion of step c with 450-500nm blue light to make the emulsion undergo polymerization reaction to obtain mosquito repellent microcapsule emulsion.