Preparation Method of Special-shaped Composite Fiber Suede-like Waterproof Fabric

Abstract

The invention discloses a preparation method of a special-shaped composite filament suede-like waterproof fabric, belonging to the field of functional fabrics. The preparation method includes: (1) weaving warp and weft into a fabric, wherein the warp is a special-shaped composite filament; (2) scouring, fiber opening, and alkali weight reduction of the woven fabric → pre-setting → sueding → dyeing → waterproof finishing; the specific waterproof finishing is as follows: impregnating and padding the dyed fabric with a waterproof agent emulsion; drying at a high temperature; the waterproof agent emulsion is composed of a cross-linking agent and a nano-silica modified polysiloxane emulsion mixed in a mass ratio of 1:20. The special-shaped composite filament suede-like waterproof fabric prepared by the method of the invention has a delicate surface, plump hair feeling, and is soft and smooth. The waterproof material applied on the fabric surface realizes a good waterproof effect through the combination of nano-silica and organic silicon.

Description

Technical Field

[0001] The present invention belongs to the field of functional fabrics, and particularly relates to a preparation method of a special-shaped composite fiber suede-like waterproof fabric. Background Art

[0002] The pile of natural suede is fine, dense, plump and soft, and can be used to make high-grade clothing. However, the quantity of natural suede is small and the price is high. To meet the consumption demand, textile manufacturers have developed a substitute - suede-like fabric. Most suede-like fabrics are formed by raising and sanding ultra-fine fiber fabrics through dyeing and finishing processes.

[0003] The diameter of ultra-fine fibers is small, and the diffuse reflection of light by the fibers increases, reducing the color depth of the fabric and resulting in poor deep dyeing property. When dyeing, more dyes need to be added to ultra-fine fiber fabrics than ordinary fibers to obtain the same dyeing depth.

[0004] Composite fibers are an important category of differential fibers. Each single fiber or fiber bundle of a composite fiber contains two or more different components, and the single fibers can be split into finer multi-filament special-shaped fibers by physical or chemical methods during subsequent processing. Fabrics woven with special-shaped fibers are opened by dissolving part of the fibers with lye and then sanded to obtain suede-like fabrics. The suede-like fabric is soft and delicate, has an obvious wool-like feel, and has a large surface area, good dyeing property, and can be dyed dark colors. Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation method of a special-shaped composite fiber suede-like waterproof fabric.

[0006] To achieve the above purpose, the present invention adopts the following technical solutions.

[0007] A preparation method of a special-shaped composite fiber suede-like waterproof fabric includes the following steps:

[0008] (1) Weaving warp and weft into a fabric, where the warp is a special-shaped composite fiber;

[0009] (2) The woven fabric is subjected to scouring, fiber opening, caustic weight reduction → pre-setting → sanding → dyeing → waterproof finishing;

[0010] The specific waterproof finishing is as follows: impregnating the dyed fabric with a waterproof agent emulsion; drying at high temperature;

[0011] The waterproof agent emulsion is composed of a cross-linking agent and a nano-silica modified polysiloxane emulsion mixed in a mass ratio of 1:20.

[0012] The warp is 11D / 84F orange petal-shaped special-shaped composite fiber.

[0013] The weft is 100D / 36F DTY.

[0014] The scouring, fiber opening, and alkali deweighting are specifically as follows: the fabric is kept at 100°C for 30 min in the treatment bath; the treatment bath formulation is 10 g / L of sodium hydroxide, 2 g / L of scouring agent, and 2 g / L of chelating dispersant; the bath ratio of the treatment bath is 1:10.

[0015] The pre-setting is carried out at a temperature of 180 - 210°C for 25 - 45 s.

[0016] For the sueding, the sandpaper is 100 mesh, the speed is 15 - 20 m / min, the wrap angle is 10 - 15 cm, and the rotational speed is 2000 - 2200 r / min.

[0017] The dyeing process is as follows: at room temperature, bath softener, leveling agent, chelating dispersant, and acetic acid are added to the bath, and it is run for 15 min. Then, the pre-dissolved disperse dye is added, and it is run for 15 min. The dye bath is heated to 85°C at a heating rate of 1.5°C / min and kept running for 30 min. Then, the dye bath is heated to 130°C at a heating rate of 0.5°C / min and dyed for 45 min. Finally, it is cooled at a speed of 1.5°C / min until the dye bath temperature drops below 50°C, and the liquid is drained.

[0018] The special-shaped composite fiber suede-like waterproof fabric prepared by the method of the present invention has a delicate surface, plump wool feeling, softness, and smoothness; the texture of the special-shaped composite fiber is fine, there are microporous structures between the fabrics, which can form a good heat insulation and warming effect; the waterproof material applied on the fabric surface is combined with nano-silicone to achieve a good waterproof effect. In addition, the ultra-fine fiber has a large specific surface area, and the fiber voids are numerous and dense, improving the self-cleaning performance of the fabric. Detailed implementation mode

[0019] The present invention discloses a preparation method of a special-shaped composite fiber suede-like waterproof fabric, comprising the following steps:

[0020] (1) The warp and weft are woven into a fabric, and the warp is a special-shaped composite fiber.

[0021] (2) The woven fabric is processed through the processes of scouring, fiber opening, alkali deweighting → pre-setting → sueding → dyeing → waterproof finishing.

[0022] The warp is 11D / 84F orange-petal-shaped special-shaped composite fiber with a density of 56 roots / cm; the weft is 100D / 36F DTY with a density of 35 roots / cm.

[0023] According to the comprehensive performance requirements of the fabric, the warp can be set as a special-shaped composite fiber, or the weft can be set as a special-shaped composite fiber, or both the warp and weft can be set as special-shaped composite fibers, and accordingly, the warp and weft densities of the fabric, the subsequent dyeing and finishing processes, and parameters are adjusted.

[0024] For the scouring, fibrillation, and alkali weight reduction, the fabric is kept at 100°C for 30 min in the treatment bath. The treatment bath formulation is 10 g / L of sodium hydroxide, 2 g / L of scouring agent, and 2 g / L of chelating dispersant. The bath ratio of the treatment bath is 1:10.

[0025] The fibrillation and alkali weight reduction treatment disperses and fluffs up the filament bundles of the originally bonded ultrafine fibers into ultrafine fiber monofilaments.

[0026] For the pre-setting, the temperature is 180 - 210°C and the time is 25 - 45 s.

[0027] The sueding mentioned is the key process for the fabric to form the suede-like appearance and style with short, dense, and uniform villi. During sueding, a 100-mesh sandpaper is used, the speed is 15 - 20 m / min, the wrap angle is 10 - 15 cm, and the rotational speed is 2000 - 2200 r / min.

[0028] For the dyeing, the technological process is as follows: At room temperature, add bath softener, leveling agent, chelating dispersant, and acetic acid to the bath, run for 15 min, then add the pre-dissolved disperse dye and run for 15 min. Heat the dye bath to 85°C at a heating rate of 1.5°C / min and keep it running for 30 min. Then heat the dye bath to 130°C at a heating rate of 0.5°C / min and keep it for dyeing for 45 min. Finally, cool at a speed of 1.5°C / min until the dye bath temperature drops below 50°C, and drain the liquid.

[0029] Dyeing process formulation:

[0030]

[0031] For the waterproof finishing, the specific process is as follows:

[0032] a. Prepare the waterproof agent emulsion;

[0033] b. Pad the dyed fabric with the waterproof agent emulsion, two-padding and two-rolling, with a liquor pickup rate of 80%;

[0034] c. Dry at 200°C.

[0035] The waterproof agent emulsion is composed of a crosslinking agent and a nano-silica modified polysiloxane emulsion in a mass ratio of 1:20. When in use, slowly add the crosslinking agent to the nano-silica modified polysiloxane emulsion and stir to mix them evenly.

[0036] The nano-silica modified polysiloxane emulsion is formed by the reaction of the thiol group with the "C=C" on the side chain of the amino-terminated vinyl polysiloxane. The low surface energy of the silicone and the nano-silica cooperate to form a hydrophobic surface.

[0037] The crosslinking agent is a water-based blocked polyurethane, a commercially available product, such as the water-based blocked isocyanate curing agent BL5335 from Covestro Germany.

[0038] The film-forming property of the nano-silica modified polysiloxane emulsion on the fabric surface is poor. After several washes of the fabric, the waterproof performance decreases significantly. The crosslinking agent is a temporarily blocked isocyanate polymer. After being thermally deblocked, the isocyanate groups can react with the amino groups in the nano-silica modified polysiloxane and the hydroxyl groups generated on the fiber surface after the fabric alkali weight reduction, playing a role in crosslinking the fabric and the polysiloxane, thereby improving the durability of functions such as the waterproofness of the fabric.

[0039] The nano-silica modified polysiloxane emulsion described above is prepared by the following steps:

[0040] ① Add amino-terminated vinyl polysiloxane, surface-modified nano-silica, photocatalyst DMPA (benzoin dimethyl ether), and freshly distilled THF (tetrahydrofuran) to the reactor in sequence. After the reactants are dissolved, keep stirring and irradiate under ultraviolet light for 30 min. After the reaction is completed, remove THF under vacuum, and precipitate the reaction product three times in anhydrous methanol to remove unreacted raw materials and catalysts, thus obtaining nano-silica modified polysiloxane; the molar ratio of the “-C=C” group in the amino-terminated vinyl polysiloxane to the “-SH” group in the surface-modified nano-silica is 1:1.05;

[0041] ② Mix the nano-silica modified polysiloxane and the emulsifier at a mass ratio of 10:1. During stirring, add a mixture of water and acetic acid, and stir until the solution becomes transparent to obtain the nano-silica modified polysiloxane emulsion. The mass percentage concentration of the emulsion is about 10%, and the emulsion is adjusted to be acidic by acetic acid. The emulsifier is composed of isomeric tridecyl alcohol polyoxyethylene ether 1307 and 1309 at a mass ratio of 1:2. The reaction process is shown in the following formula (1).

[0042]

[0043] Among them, the preparation method of the amino-terminated vinyl polysiloxane is:

[0044] In a dry four-necked flask equipped with a thermometer and a stirrer, add 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, octamethylcyclotetrasiloxane, and tetramethyltetravinylcyclotetrasiloxane with a molar ratio of 1:40:2. While stirring, heat up to the reaction temperature, and add a certain amount of trifluoromethylsulfonic acid, and keep the reaction at a certain temperature for a certain time; after the reaction is completed, add anhydrous Na 2 CO 3Stir and neutralize to pH 6 - 7, filter and subject the product to vacuum distillation (90 °C, vacuum below -0.1 Mpa) to remove unreacted monomers, obtaining a colorless and transparent liquid product, which is an amino-terminated vinyl polysiloxane. The conversion rate is 91.5%, M n (g / mol): 12776, the C=C bond content is 0.626 mmol / g; the reaction process is as shown in reaction formula (2).

[0045]

[0046] The surface-modified nano-silica described above has a preparation method as follows:

[0047] Weigh an appropriate amount of nano-SiO 2 Add it to absolute ethanol, and use magnetic stirring to make nano-SiO 2 Disperse evenly, adjust the pH value to 4 with HCl solution, then dropwise add the silane coupling agent KH590 (γ-mercaptopropyltrimethoxysilane) to the system. After mixing evenly, transfer the solution to a three-necked flask, control the system temperature at 80 °C, stir and react for 10 h, cool, filter, wash, and dry the mixed solution to obtain KH590 surface-modified nano-Si0 2 . The mass ratio of nano-SiO 2 , silane coupling agent KH590, and absolute ethanol is 10:1.5:100. The relative grafting rate of the silane coupling agent on the surface of nano-SiO 2 is about 10%. ● represents nano-silica. The reaction process is as shown in reaction formula (3).

[0048]

[0049] Example 1:

[0050] A special-shaped composite filament fabric is woven from warp and weft. Among them, the warp is 11D / 84F orange-petal-shaped special-shaped composite filament with a density of 56 roots / cm; the weft is 100D / 36F DTY with a density of 35 roots / cm; it is a five-harness three-fly warp satin weave.

[0051] The production process flow of the fabric:

[0052]

[0053] Example 2:

[0054] A preparation method of a special-shaped composite filament suede-like waterproof fabric includes the following steps:

[0055] (1) Weave the warp and weft into a fabric, as shown in Example 1;

[0056] (2) The woven fabric is subjected to scouring, fiber opening, caustic weight reduction → pre-setting → sueding → dyeing → waterproof finishing;

[0057] ① Scouring, fiber opening, caustic weight reduction:

[0058] The process conditions and formulation are as follows

[0059] Sodium hydroxide 10 g / L

[0060] Scouring agent 2 g / L

[0061] Chelating dispersant 2 g / L

[0062] Bath ratio 1:10

[0063] Temperature 100 °C

[0064] Time 30 min

[0065] Add sodium hydroxide, scouring agent, and chelating dispersant to the water bath, run for 10 min, immerse the fabric, run for 15 min, heat the dye bath to 100 °C at a heating rate of 1 °C / min, hold for 30 min, then cool to below 50 °C at a rate of 1.5 °C / min, drain the liquid, neutralize with acetic acid, and wash until neutral.

[0066] ② Pre-setting: Temperature is 180 - 210 °C, time is 25 - 45 s, and vehicle speed is 25 - 40 m / min.

[0067] ③ Sueding: Use 100-mesh sandpaper, fabric speed is 15 - 20 m / min, wrap angle is 10 - 15 cm, and cylinder rotation speed is 2000 - 2200 r / min.

[0068] ④ Dyeing:

[0069] The formulation and process conditions are as follows:

[0070]

[0071] At room temperature, add bath softener, leveling agent, chelating dispersant, and acetic acid to the dye bath, run for 15 min, then add the pre-dissolved disperse dye, run for 15 min, heat the dye bath to 85 °C at a heating rate of 1.5 °C / min, hold for 30 min, then heat the dye bath to 130 °C at a heating rate of 0.5 °C / min and hold for 45 min for dyeing; finally, cool at a rate of 1.5 °C / min until the dye bath temperature drops below 50 °C, and drain the liquid.

[0072] To improve the color fastness of the fabric after dyeing, for medium and dark colors, a reduction cleaning step can be added after dyeing. The formulation and process conditions for reduction cleaning are: sodium hydrosulfite 2 g / L, soda ash 2 g / L, liquor ratio 1:10, temperature 85 °C, time 10 min. After discharging the wastewater, neutralize with acetic acid and wash the fabric with clear water until the pH value is neutral.

[0073] ⑤ Waterproof finishing:

[0074] a. Mix the waterborne blocked isocyanate curing agent BL5335 and the nano-silica modified polysiloxane emulsion in a mass ratio of 1:20, stir evenly, and prepare a waterproof agent emulsion;

[0075] b. Pad the dyed fabric with the waterproof agent emulsion, two-padding and two-rolling, and the liquor pickup rate is about 80%;

[0076] c. Dry at 200 °C for 30 - 40 s, with a vehicle speed of 25 - 40 m / min.

[0077] The relevant properties of the obtained special-shaped composite filament suede-like waterproof fabric were tested, and the results were: water repellency was 5 grades before washing and 4 grades after 5 washes; soaping color fastness ≥ 3 grades; water color fastness ≥ 3 grades; rubbing color fastness ≥ 3 grades.

[0078] The water repellency performance test was carried out with reference to GB / T 4745-2012 "Textiles - Determination of waterproof performance - Spray test"; the soaping color fastness test was carried out with reference to GB / T 3921-2008 "Textiles - Tests for color fastness - Color fastness to soaping"; the water color fastness test was carried out with reference to GB / T 5713-2013 "Textiles - Tests for color fastness - Color fastness to water"; the rubbing color fastness test was carried out with reference to GB / T 3920-2008 "Textiles - Tests for color fastness - Color fastness to rubbing".

Claims

1. Preparation method of a special-shaped composite filament suede-like waterproof fabric, which comprises the following steps: (1) Warp and weft are woven into a fabric, and the warp is a special-shaped composite filament; (2) The woven fabric is scoured, defibrated, alkali-deweighted → pre-set → sueding → dyed → waterproof finished; The specific waterproof finishing is as follows: The dyed fabric is padded with a waterproof agent emulsion; dried at high temperature; The waterproof agent emulsion is composed of a cross-linking agent and a nano-silica modified polysiloxane emulsion mixed in a mass ratio of 1:20; The warp is 11D / 84F orange petal-shaped special-shaped composite filament; The weft is 100D / 36F DTY; The nano-silica modified polysiloxane emulsion is prepared by the following steps: ① Add amino-terminated vinyl polysiloxane, surface-modified nano-silica, photo-catalyst DMPA (benzoin dimethyl ether) and freshly distilled THF (tetrahydrofuran) to the reactor in sequence. After the reactants are dissolved, keep stirring and irradiate under ultraviolet light for 30 min. After the reaction is completed, vacuum remove THF, and precipitate the reaction product three times in anhydrous methanol to remove unreacted raw materials and catalysts, thus obtaining nano-silica modified polysiloxane; the molar ratio of the "-C=C" group in the amino-terminated vinyl polysiloxane to the "-SH" group in the surface-modified nano-silica is 1:1.05; ② Mix the nano-silica modified polysiloxane and an emulsifier in a mass ratio of 10:1, add a mixture of water and acetic acid during stirring, and stir until the solution becomes transparent to obtain a nano-silica modified polysiloxane emulsion; The preparation method of the amino-terminated vinyl polysiloxane is: In a dry four-necked flask equipped with a thermometer and a stirrer, add 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, octamethylcyclotetrasiloxane, and tetramethyltetravinylcyclotetrasiloxane with a molar ratio of 1:40:

2. While stirring, heat up to the reaction temperature, and add a certain amount of trifluoromethanesulfonic acid. Keep the reaction at a certain temperature for a certain time. After the reaction is completed, add anhydrous Na 2 CO 3 Stir and neutralize to a pH of 6-7, filter, and subject the product to vacuum distillation to remove unreacted monomers, obtaining a colorless transparent liquid product, which is an amino-terminated vinyl polysiloxane.

2. The preparation method of a special-shaped composite filament suede-like waterproof fabric according to claim 1, characterized in that: For the scouring, defibrating, and alkali-deweighting, the prescription and specific process conditions are that the fabric is kept at 100 °C for 30 min in the treatment bath; the treatment bath prescription is 10 g / L of sodium hydroxide, 2 g / L of scouring agent, and 2 g / L of chelating dispersant; the bath ratio of the treatment bath is 1:

10.

3. The preparation method of a special-shaped composite filament suede-like waterproof fabric according to claim 1, characterized in that: For the pre-set, the specific process conditions are a temperature of 180 - 210 °C and a time of 25 - 45 s.

4. The preparation method of a special-shaped composite filament suede-like waterproof fabric according to claim 1, characterized in that: For the sueding, the specific process conditions are 100-mesh sandpaper, a speed of 15 - 20 m / min, a wrap angle of 10 - 15 cm, and a rotational speed of 2000 - 2200 r / min.

5. The preparation method of a special-shaped composite filament suede-like waterproof fabric according to claim 1, characterized in that: For the described dyeing, the technological process is as follows: at room temperature, add softener, leveling agent, chelating dispersant, and acetic acid to the bath, run for 15 minutes, then add the pre-dissolved disperse dye and run for 15 minutes. Heat the dye bath to 85°C at a heating rate of 1.5°C / min, keep it warm and run for 30 minutes, then heat the dye bath to 130°C at a heating rate of 0.5°C / min and keep it warm for dyeing for 45 minutes; finally, cool at a speed of 1.5°C / min, cool the dye bath to below 50°C, and drain the liquid.

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