Preparation method of bio-based nylon composite fabric

Abstract

The invention discloses a preparation method of a bio-based nylon composite fabric. The preparation method comprises the following steps: padding a base material fabric in a phosphorus-containing quaternary ammonium salt organosiloxane solution; soaking a base material fabric in the waterproof finishing liquid, mangling, pre-drying and baking; the base material fabric and the functional film are compounded, and the bio-based nylon composite fabric is prepared; the phosphorus-containing quaternary ammonium salt organosiloxane solution is prepared from phosphorus-containing quaternary ammonium salt organosiloxane, ethanol and water. The method comprises the following steps: firstly finishing a base material fabric with a phosphorus-containing quaternary ammonium salt organosiloxane solution to enable the fabric to form a flame-retardant function, then carrying out waterproof finishing on the fabric, and then compounding the base material fabric with a functional film to prepare the fabric with the properties of flame retardance, water resistance, moisture permeability and the like. The phosphorus-containing quaternary ammonium salt organosiloxane has quaternary ammonium cation adsorption and siloxy condensation, so that the organosiloxane is firmly attached to the fibers and does not migrate, the fabric has flame retardant property, and the flame retardant durability can be enhanced.

Description

Technical Field

[0001] The present invention relates to a preparation method of a bio-based nylon composite fabric, belonging to the field of functional textile fabrics. Background Art

[0002] Bio-based nylon is a new synthetic fiber material with important application potential, and it has significant advantages in terms of environmental friendliness, sustainability and functionality. As a sustainable alternative to traditional synthetic fibers, bio-based nylon fabrics have attracted much attention from the research and industrial communities. Currently, synthetic fiber materials are widely used in the textile industry, but their preparation processes usually rely on non-renewable petroleum resources and also generate a large amount of harmful waste. In order to reduce the adverse impact on the environment, finding substitutes has become an urgent need. Bio-based nylon, as a sustainable synthetic fiber material, has been widely studied and developed.

[0003] The waterproof and moisture-permeable composite fabric has good waterproofness, good air permeability and moisture permeability. The water vapor in the human body can be dissipated in time, without giving people an abnormally stuffy feeling. Even under cold outdoor conditions, it will not cause sweat to accumulate and condense on the fabric surface, giving people a cold feeling. Such composite fabrics can meet the requirements of consumers for wearing comfort. Summary of the Invention

[0004] The purpose of the present invention is to provide a preparation method of a bio-based nylon composite fabric, which first applies a flame retardant and waterproof agent on the surface of the bio-based nylon base fabric, and then composites it with a functional film to make a fabric with functions such as flame retardancy, waterproofness and moisture permeability.

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

[0006] A preparation method of a bio-based nylon composite fabric includes the following steps:

[0007] The base fabric is impregnated and rolled with a phosphonium quaternary ammonium salt organosiloxane solution;

[0008] The base fabric is immersed in a waterproof finishing solution, rolled, pre-baked and baked;

[0009] The base fabric is composited with a functional film to make a bio-based nylon composite fabric;

[0010] The phosphonium quaternary ammonium salt organosiloxane solution is composed of phosphonium quaternary ammonium salt organosiloxane, ethanol and water;

[0011] The preparation method of the phosphonium quaternary ammonium salt organosiloxane is as follows:

[0012] 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;

[0013] 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.

[0014] The substrate fabric is dipped into a phosphorus-containing quaternary ammonium salt organic siloxane solution, and the specific steps are: preparing a 12wt% phosphorus-containing quaternary ammonium salt organic siloxane ethanol / water solution (ethanol / water volume ratio 60:40), adjusting the solution pH to 5-5.5, putting the substrate fabric into the solution for immersion reaction for 30 minutes, and then taking out the substrate fabric and drying it.

[0015] The waterproof finishing liquid is composed of a waterproofing agent, water and a cross-linking agent. By mass volume, the waterproofing agent is 50 g / L and the cross-linking agent is 10 g / L.

[0016] Waterproof finishing process:

[0017] The base fabric is immersed in the waterproof agent finishing liquid (two immersions and two rollings, the rolling rate is 50-60%) → pre-baking (100°C, 2min) → baking (150°C, 30s).

[0018] The waterproofing agent is fluorine-free environmentally friendly waterproofing agent Furex-5779.

[0019] The functional film is a polyurethane TPU film with a thickness of 0.012 mm.

[0020] The substrate fabric and the functional film are laminated in the following specific steps:

[0021] ① Gluing: First apply glue dots on the surface of the base fabric and functional film.

[0022] ② Lamination: The fabric and the film are stacked together flatly, and then moved to the pressing machine, and then the hot pressing time and hot pressing temperature are set. After the temperature is reached, pressing is carried out to complete the hot pressing lamination and make bio-based nylon composite fabric.

[0023] A preparation method of a bio-based nylon composite fabric disclosed by the present invention first uses a phosphonium quaternary ammonium salt organosiloxane solution to finish the bio-based nylon substrate fabric to endow the fabric with a flame retardant function, then performs waterproof finishing on the fabric, and then composites the substrate fabric with a functional film to produce a fabric with properties such as flame retardancy, waterproofness, and moisture permeability.

[0024] The flame retardants and waterproofing agents used in the flame retardant and waterproof finishing of textiles are usually hydrophilic and hydrophobic respectively. If the flame retardant and waterproofing agents are mixed and finished in one bath, they are likely to be immiscible due to physical property differences; if the two-bath step-by-step finishing method is adopted, the former finishing will affect the latter, affecting the flame retardant and waterproof functions of the fabric. The fluorine-free waterproofing agent adopted by the present invention is an organosilicon compound, which has good compatibility with the phosphonium quaternary ammonium salt organosiloxane, and can also undergo a cross-linking reaction with each other to enhance the binding force between the two; the flame retardant and waterproof finishing are carried out step by step, and according to the needs of the flame retardant and waterproof properties, the dosages of the flame retardant and waterproof finishing agents can be adjusted respectively without causing a deteriorating effect on each other.

[0025] The adsorption of the organosilicon quaternary ammonium cation and the condensation of the silane oxy groups in the phosphonium quaternary ammonium salt organosiloxane enable the organosiloxane to firmly adhere to the fiber, and its non-migratory property enhances the durability of the flame retardancy. Specific embodiments

[0026] The technical solution of the present invention will be described in detail below through specific examples.

[0027] The present invention discloses a preparation method of a bio-based nylon composite fabric, including the following steps:

[0028] The bio-based nylon substrate fabric is impregnated and rolled with a phosphonium quaternary ammonium salt organosiloxane solution;

[0029] The bio-based nylon substrate fabric is immersed in a waterproof finishing solution, rolled, pre-baked, and baked;

[0030] The bio-based nylon substrate fabric is composited with a functional film to produce a composite fabric;

[0031] The phosphonium quaternary ammonium salt organosiloxane solution is composed of a phosphonium quaternary ammonium salt organosiloxane, ethanol, and water;

[0032] The preparation method of the phosphonium quaternary ammonium salt organosiloxane is as follows:

[0033] 17.3 g of diethyl chlorophosphate and 50 mL of tetrahydrofuran are added to the S1 reactor, and nitrogen is introduced for protection at the same time. Then 9 g of N,N-dimethylethanolamine and 3 g of triethylamine are added and stirred and reacted in an ice-water bath for 4 h. After the reaction is complete, the organic solvent tetrahydrofuran is removed by vacuum distillation, and suction filtration is carried out to obtain (triethyl phosphate)N,N-dimethylamine;

[0034] 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.

[0035] The reaction formula for preparing phosphorus-containing quaternary ammonium salt organosiloxane is as follows:

[0036]

[0037] The substrate fabric is dipped into a phosphorus-containing quaternary ammonium salt organic siloxane solution, and the specific steps are: preparing a 12wt% phosphorus-containing quaternary ammonium salt organic siloxane ethanol / water solution (ethanol / water volume ratio 60:40), adjusting the solution pH to 5-5.5, putting the substrate fabric into the solution for immersion reaction for 30 minutes, and then taking out the substrate fabric and drying it.

[0038] The waterproof finishing liquid is composed of a waterproofing agent, water, and a crosslinking agent, wherein the waterproofing agent is 50 g / L and the crosslinking agent is 10 g / L by mass volume. The waterproofing agent and the crosslinking agent are products of Mingren Fine Chemicals (Jiaxing) Co., Ltd., which are fluorine-free environmentally friendly waterproofing agent Furex-5779 and crosslinking agent 3701, respectively.

[0039] Waterproof finishing process:

[0040] The base fabric is immersed in the waterproof finishing liquid (two immersions and two rollings, the rolling rate is 50-60%) → pre-baking (100° C., 2 min) → baking (150° C., 30 s).

[0041] The functional film is a polyurethane TPU film with a thickness of 0.012 mm. The functional film gives the composite fabric good moisture permeability, air permeability and hydrostatic pressure resistance.

[0042] The substrate fabric and the functional film are laminated in the following specific steps:

[0043] ① Glue coating: first apply glue dots on the surface of the base fabric and functional film, with the amount of glue applied being 25-30g / m 2 ;

[0044] ② Lamination: The fabric and the film are stacked together flatly, and then moved to the pressing machine, and then the hot pressing temperature is set to 105℃ and the hot pressing time is set to 30s. After the temperature is reached, pressing is performed, the winding pressure is 3kg, and the laminating speed is 10m / min. The hot pressing lamination is completed to make a bio-based nylon composite fabric.

[0045] The adhesive is polyurethane hot melt adhesive, which is a conventional product available on the market.

[0046] The bio-based nylon base fabric used in the example has warp and weft threads: 40D / 36F + 20DSP * 40D / 36F + 20DSP, composition: 89% bio-based nylon + 11% spandex, warp and weft density: 86×64.

[0047] Before the bio-based nylon base fabric is impregnated with the quaternary ammonium salt organosiloxane solution containing phosphorus, it needs to undergo conventional pretreatment before scouring to remove surface oil stains and facilitate subsequent functional finishing.

[0048] Pretreatment before scouring of the base fabric: The base fabric is put into the pretreatment liquid → heated to 100 °C and kept warm for 30 min → cooled and washed with water; the pretreatment liquid contains 4 g / L soda ash, 2 g / L scouring agent, 2 g / L chelating dispersant, and the rest is water, and the liquor ratio is 1:8.

[0049] The scouring agent, chelating dispersant, etc. involved in the pretreatment steps before scouring are all commercially available conventional products.

[0050] Example 1:

[0051] Preparation method of the bio-based nylon composite fabric:

[0052] 1), Mix ethanol / water in a volume ratio of 60:40, then add the quaternary ammonium salt organosiloxane containing phosphorus to prepare a 12 wt% solution, adjust the pH of the solution to 5 - 5.5, put the bio-based nylon base fabric into the solution for impregnation reaction for 30 min, then take out the base fabric and dry it at 100 °C for 60 s;

[0053] 2), The fluorine-free environmentally friendly waterproof agent Furex-5779, cross-linking agent 3701 and water are formulated into a waterproof finishing liquid. By mass-volume, the waterproof agent in the finishing liquid is 50 g / L and the cross-linking agent is 10 g / L; the waterproof finishing process flow is that the base fabric is impregnated in the waterproof finishing liquid (two dips and two nips, nip ratio 50 - 60%) → pre-drying (100 °C, 2 min) → curing (150 °C, 30 s);

[0054] 3), The base fabric is compounded with the functional film. The specific steps are as follows:

[0055] ① Glue coating: First, apply glue dots on the surfaces of the base fabric and the functional film. The glue is polyurethane hot melt glue, and the coating amount is 25 - 30 g / m 2 ;

[0056] ② Film laminating: The fabric and the film are stacked flat together, then moved to a hot press, and then set the hot press temperature to 105 °C and the hot press time to 30 s. After the temperature reaches, perform hot pressing, the winding pressure is 3 kg, and the laminating speed is 10 m / min to complete the hot press laminating and make the bio-based nylon composite fabric.

[0057] The flame retardancy, water resistance and other properties of the bio-based nylon composite fabric prepared by the method of the embodiment were tested.

[0058] Flame retardancy of the bio-based nylon composite fabric: Afterflame time is 2 s, smoldering time is 1 s, char length is 9.4 cm. The flame retardancy test refers to "GB / T 5455-2014 Textiles - Determination of burning behavior - Vertical burning method, afterflame and smoldering times, and char length".

[0059] Waterproof and moisture-permeable properties of the bio-based nylon composite fabric:

[0060] Hydrostatic pressure resistance: 13760 mmH 2 O before washing, 9020 mmH 2 O after 20 washes. The test method refers to

[0061] "GB / T 4744-2013 Textiles - Determination of water resistance - Hydrostatic pressure test".

[0062] Moisture permeability: 7170 g·m -2 ·24 h -1 , and the test method refers to "GB / T 12704.1-2009 Textiles - Test methods for fabric moisture permeability - Part 1: Moisture absorption method".

[0063] Water repellency grade: Grade 4-5 before washing, Grade 3-4 after 20 washes. The test method refers to "GB / T 4745-2012 Textiles - Determination of water repellency - Spray test".

Claims

1. A preparation method of a bio-based nylon composite fabric, comprising the following steps: The bio-based nylon base fabric is padded with a phosphonium quaternary ammonium salt organosiloxane solution; The bio-based nylon base fabric is impregnated in a waterproof finishing solution, padded, pre-dried, and baked; The bio-based nylon base fabric is compounded with a functional film to make a bio-based nylon composite fabric; The phosphonium quaternary ammonium salt organosiloxane solution is composed of a phosphonium quaternary ammonium salt organosiloxane, ethanol, and water; The preparation method of the phosphonium quaternary ammonium salt organosiloxane is as follows: S1: Add 17.3 g of diethyl chlorophosphate and 50 mL of tetrahydrofuran to the reactor, and at the same time introduce nitrogen for protection. Then continue to add 9 g of N,N-dimethylethanolamine and 3 g of triethylamine and stir and react in an ice-water bath for 4 h. After the reaction is complete, perform vacuum distillation to remove the organic solvent tetrahydrofuran, and filter 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 and react at 70 °C. After the reactants become transparent, react for another 2 hours, and then remove isopropanol under the condition of 0.01 MPa to obtain a viscous liquid, which is the phosphonium quaternary ammonium salt organosiloxane.

2. The preparation method of a bio-based nylon composite fabric according to claim 1, characterized in that: For the base fabric to be padded with the phosphonium quaternary ammonium salt organosiloxane solution, the specific steps are: prepare a 12 wt% phosphonium quaternary ammonium salt organosiloxane ethanol / water solution, adjust the pH of the solution to 5-5.5, immerse the base fabric in the solution for reaction for 30 min, and then take out the base fabric and dry it.

3. The preparation method of a bio-based nylon composite fabric according to claim 1, characterized in that: The waterproof finishing solution is composed of a waterproof agent, water, and a cross-linking agent. Calculated by mass volume, the waterproof agent is 50 g / L and the cross-linking agent is 10 g / L.

4. The preparation method of a bio-based nylon composite fabric according to claim 1, characterized in that: The waterproof finishing process flow is to impregnate the base fabric in the waterproof agent finishing solution, pad → pre-dry → bake.

5. The preparation method of a bio-based nylon composite fabric according to claim 1, characterized in that: The functional film is a polyurethane TPU film with a thickness of 0.012 mm.

6. The preparation method of a bio-based nylon composite fabric according to claim 1, characterized in that, For the compounding of the base fabric and the functional film, the specific steps are: ① Glue coating: First, apply glue dots on the surfaces of the base fabric and the functional film, ② Film laminating: The fabric and the film are stacked flat together, then moved to a hot press, and then set the hot pressing time and hot pressing temperature. After the temperature reaches, perform hot pressing to complete hot press film laminating to make a bio-based nylon composite fabric.

Images