Short-process dyeing and finishing process for anti-ultraviolet flame-retardant cotton fabric

Abstract

The invention discloses a short-process dyeing and finishing process for an anti-ultraviolet flame-retardant cotton fabric. The short-process dyeing and finishing process comprises the following specific steps: (1) performing cold pad-batch pretreatment on the cotton fabric; the cold pad-batch pretreatment of the cotton fabric specifically comprises the steps of padding in a working solution, rolling and wrapping, piling, washing with hot water at 95 DEG C and drying; (2) dyeing; the method comprises the specific steps of cloth feeding, dye liquor padding, drying, color fixing liquor padding, steaming color fixing, soaping and drying. (3) finishing the functional coating slurry; the functional coating slurry is prepared from a POSS (Polyhedral Oligomeric Silsesquioxane)-based acrylate emulsion, a thickening agent and water; stirring a POSS-based acrylate emulsion, a thickening agent and water to form functional coating slurry; the fabric is padded with functional coating slurry, two times of dipping and two times of rolling are carried out, and the mangle expression is 70%-80%; and pre-drying and baking to obtain the anti-ultraviolet flame-retardant cotton fabric. The dyeing and finishing process of the cotton fabric is energy-saving and consumption-reducing, and the fabric has good anti-ultraviolet and flame-retardant properties.

Description

Technical Field

[0001] This invention belongs to the field of functional textile dyeing and finishing, specifically relating to a short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics. Background Technology

[0002] Cotton fabrics are soft and gentle on the skin, absorbent and breathable, making people feel comfortable. Cotton's natural environmental friendliness, absence of parasites and bacteria, and lack of static electricity also make it excellent in terms of warmth and health. Pure cotton fabrics have a natural affinity for the skin, making them one of the most basic and reliable textiles in daily life. However, the dyeing and finishing process for cotton fabrics is lengthy, time-consuming, and energy-intensive, requiring environmentally friendly and green processing methods. Summary of the Invention

[0003] The purpose of this invention is to provide a short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics.

[0004] To achieve the above objectives, the present invention adopts the following technical solution.

[0005] A short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics, comprising the following steps: (1) Pretreatment of cotton fabrics before cold pad-batch processing; (2) Staining; (3) Finishing of functional coating paste; The functional coating paste is composed of POSS-based acrylate emulsion, thickener, and water.

[0006] The pretreatment of cotton fabrics before cold pad-batch processing is specifically as follows: padding with working solution → rolling and wrapping → stacking → washing with hot water at 95℃ → drying.

[0007] The working solution, by weight / volume, contains 12 g / L hydrogen peroxide, 40 g / L caustic soda, 9 g / L oxygen bleaching stabilizer, 16 g / L refining agent, 2 g / L chelating agent, 2 g / L penetrant, and the remainder is water.

[0008] The POSS-based acrylate emulsion is prepared by emulsion polymerization of OvPOSS, phosphorus nitrogen-based acrylate flame retardant monomers, 2-hydroxy-4-methacryloyloxybenzophenone, butyl acrylate, styrene, methyl methacrylate, emulsifier, initiator, and water.

[0009] The POSS-based acrylate emulsion is prepared by the following method: Add 200 parts deionized water, 8 parts OvPOSS, 16 parts phosphorus nitrogen acrylate flame retardant monomer, 5 parts 2-hydroxy-4-methacryloyloxybenzophenone, 60 parts butyl acrylate, 10 parts styrene, 18 parts methyl methacrylate, 3 parts cetyltrimethylammonium bromide, and 5 parts nonylphenol polyoxyethylene ether to an emulsifier, and emulsify at high speed for 30 minutes to obtain a pre-emulsion; Dissolve 1.3 parts of azobisisobutyramidine hydrochloride initiator in 20 parts of deionized water to prepare an initiator solution; Add the remaining 160 parts of deionized water and 1 / 3 of the pre-emulsion to the reactor, stir, and purge the air with nitrogen for 15 minutes; slowly raise the temperature to 75±1℃, and add about 1 / 3 of the initiator solution to the reactor; maintain the temperature and react for about 30 minutes; at the same time, start adding the remaining pre-emulsion and the remaining initiator solution dropwise; after the dropwise addition is complete, raise the temperature of the reaction system to 80℃ and continue to keep the reaction at this temperature for 1 hour; Stop heating and slowly cool to below 40°C; adjust the pH of the emulsion to 5.0-6.0 with dilute acetic acid solution to obtain POSS-based acrylate emulsion.

[0010] The thickener is a nonionic thickener, a commercially available product, such as DM-5329 (Demei Chemical).

[0011] The cotton fabric dyeing and finishing process of this invention completes desizing, scouring and bleaching with cold pad-batch pretreatment, which has extremely low energy consumption, flexible process and minimal fabric damage.

[0012] The POSS in the acrylate emulsion of this invention is a rigid, cage-like inorganic nanoframework composed of silicon-oxygen bonds. When POSS is uniformly dispersed in the polymer matrix, these tiny inorganic nanoparticles can effectively scatter and reflect incident ultraviolet light. POSS works synergistically with benzophenone-based UV stabilizers to significantly improve the UV protection efficiency and durability of the entire system.

[0013] POSS possesses a rigid, three-dimensional cage-like or trapezoidal inorganic silicon-oxygen framework. When uniformly dispersed in a polymer matrix, these nanoparticles effectively hinder the transfer and diffusion of heat, combustible volatile decomposition products, and oxygen. The inorganic silicon-oxygen framework (-Si-O-) structure of POSS is highly stable and not easily decomposed, promoting the rapid formation of a continuous, dense, and high-strength char layer on the burning surface of the polymer. POSS, in synergy with phosphorus-nitrogen acrylate flame-retardant monomers, can enhance the flame-retardant properties of cotton fabrics. Detailed Implementation

[0014] This invention discloses a short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics, the specific steps of which are as follows: (1) Pretreatment of cotton fabrics before cold pad-batch processing; The pretreatment of cotton fabrics before cold pad-batch processing is as follows: padding working solution (room temperature, two dips and two nips, 100% padding rate) → rolling and wrapping (sealing with plastic film to prevent drying) → stacking (room temperature, 24 hours) → washing with 95℃ hot water → drying. The working solution, by weight / volume, contains 12 g / L hydrogen peroxide, 40 g / L caustic soda, 9 g / L oxygen bleaching stabilizer, 16 g / L refining agent, 2 g / L chelating agent, 2 g / L penetrant, and the remainder is water; (2) Staining; The specific steps are as follows: feeding the fabric → padding with dye liquor (room temperature, 65%-70% padding rate) → drying → padding with fixing liquor (20 g / L soda ash, 200 g / L sodium sulfate, 65%-70% padding rate) → steam fixing (102-105℃, 2 min) → soaping (95℃, 2 g / L soaping agent, 10 min) → drying; (3) Finishing of functional coating paste; The functional coating paste is composed of POSS-based acrylate emulsion, thickener, and water; the POSS-based acrylate emulsion, thickener, and water are stirred to form the functional coating paste; the functional coating paste is applied to cotton fabric, with two dips and two nips, and the nipping rate is 70%-80%; pre-drying (90℃, 5 min) → baking (150℃, 3 min) to obtain UV-resistant flame-retardant cotton fabric.

[0015] The scouring agent, oxygen bleaching stabilizer, penetrant, soaping agent, and chelating agent are commercially available conventional products, such as scouring agent DM-1346N, oxygen bleaching stabilizer DM-1402A, penetrant DM-1221, detergent 209, and phosphorus-free chelating dispersant LS-7700, etc.

[0016] The thickener is a nonionic thickener, a commercially available product, such as DM-5329 (Demei Chemical).

[0017] The POSS-based acrylate emulsion is prepared by emulsion polymerization of OvPOSS, phosphorus nitrogen-based acrylate flame retardant monomers, 2-hydroxy-4-methacryloyloxybenzophenone, butyl acrylate, styrene, methyl methacrylate, emulsifier, initiator, and water.

[0018] The POSS-based acrylate emulsion is prepared by the following method: Add 200 parts deionized water, 8 parts OvPOSS, 16 parts phosphorus nitrogen acrylate flame retardant monomer, 5 parts 2-hydroxy-4-methacryloyloxybenzophenone, 60 parts butyl acrylate, 10 parts styrene, 18 parts methyl methacrylate, 3 parts cetyltrimethylammonium bromide, and 5 parts nonylphenol polyoxyethylene ether to an emulsifier, and emulsify at high speed for 30 minutes to obtain a pre-emulsion; Dissolve 1.3 parts of azobisisobutyramidine hydrochloride initiator in 20 parts of deionized water to prepare an initiator solution; Add the remaining 160 parts of deionized water and 1 / 3 of the pre-emulsion to the reactor, stir, and purge the air with nitrogen for 15 minutes; slowly raise the temperature to 75±1℃, and add about 1 / 3 of the initiator solution to the reactor; maintain the temperature and react for about 30 minutes; at the same time, begin to add the remaining pre-emulsion (to be added dropwise at a uniform rate over 2 hours) and the remaining initiator solution (to be added dropwise at a uniform rate over 2.5 hours); after the addition is complete, raise the temperature of the reaction system to 80℃ and continue to keep the reaction at this temperature for 1 hour; Stop heating and slowly cool to below 40°C; adjust the pH of the emulsion to 5.0-6.0 with dilute acetic acid solution to obtain POSS-based acrylate emulsion.

[0019] The OvPOSS mentioned above is prepared by the following method: 7.4 g of vinyltrimethoxysilane, 75 mL of acetone, 12.5 mL of concentrated hydrochloric acid, and 14.8 g of distilled water were weighed sequentially and added to a three-necked flask equipped with a magnetic stir bar and a condenser. The mixture was reacted at 40 °C for 24 h, during which a white precipitate was observed to gradually precipitate. After the reaction was completed, the mixture was filtered and washed several times with acetone. The solid product was then transferred to a glass dish and dried in a vacuum oven for 12 h to obtain the OvPOSS product. The yield was calculated to be 20.48%.

[0020] The phosphorus-nitrogen-based acrylate flame retardant monomer is prepared by the following method: ： Using phosphorus oxychloride as a raw material, it was dissolved in chloroform and the reaction temperature was maintained at 35°C. Neopentyl glycol was slowly added and the reaction was maintained for 4 hours. The temperature was then raised to 45°C and stirred for 1 hour, followed by a further increase to 60°C and stirring for 1 hour. After the above reaction was completed, the resulting solution was placed in a rotary evaporator to remove the solvent, thereby obtaining the intermediate 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxophosphazenecyclohexane. The purified intermediate product was dissolved with dimethylaminoethyl methacrylate in N,N-dimethylformamide, and after purging with nitrogen, it was reacted at 80°C for 24 hours in the presence of potassium iodide and a polymerization inhibitor (1,4-benzene hydroquinone). After the reaction was completed, the solution was filtered and purified. Then, it was placed in a rotary evaporator again to remove the solvent, obtaining a phosphorus-nitrogen acrylate flame retardant monomer. The molar ratio of phosphorus oxychloride, neopentyl glycol, dimethylaminoethyl methacrylate, and potassium iodide was 1.3:1.3:1:1.3. The structure is shown below.

[0021] Example 1 A short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics, comprising the following steps: (1) Pretreatment of cotton fabrics before cold pad-batch processing; The pretreatment of cotton fabrics before cold pad-batch processing is as follows: padding working solution (room temperature, two dips and two nips, 100% padding rate) → rolling and wrapping → stacking (room temperature, 24 hours) → washing with 95℃ hot water → drying. The working solution, by weight / volume, contains 12 g / L hydrogen peroxide, 40 g / L caustic soda, 9 g / L oxygen bleaching stabilizer DM-1402A, 16 g / L refining agent DM-1346N, 2 g / L phosphorus-free chelating dispersant LS-7700, 2 g / L penetrant DM-1221, with the remainder being water; (2) Staining; The specific steps are as follows: feeding the fabric → padding the cotton fabric with dye (reactive golden yellow MZ-PR, 4 g / L, room temperature, 65%-70% padding rate) → drying → padding the cotton fabric with fixative (soda ash 20 g / L, sodium sulfate 200 g / L, 65%-70% padding rate) → steam fixation (102-105℃, 2 min) → soaping (95℃, detergent 209 2 g / L, 10 min) → drying; (3) Finishing of functional coating paste; The functional coating paste is composed of POSS-based acrylate emulsion, thickener, and water; 56 parts of POSS-based acrylate emulsion, 3 parts of thickener DM-5329, and 38 parts of water are stirred to form the functional coating paste; cotton fabric is impregnated with the functional coating paste, with two impregnations and two nippings, and a nipping rate of 70%-80%; pre-drying (90℃, 5 min) → baking (150℃, 3 min) to obtain UV-resistant flame-retardant cotton fabric.

[0022] The POSS-based acrylate emulsion is prepared by the following method: Add 200 parts deionized water, 8 parts OvPOSS, 16 parts phosphorus nitrogen acrylate flame retardant monomer, 5 parts 2-hydroxy-4-methacryloyloxybenzophenone, 60 parts butyl acrylate, 10 parts styrene, 18 parts methyl methacrylate, 3 parts cetyltrimethylammonium bromide, and 5 parts nonylphenol polyoxyethylene ether to an emulsifier, and emulsify at high speed for 30 minutes to obtain a pre-emulsion; Dissolve 1.3 parts of azobisisobutyramidine hydrochloride initiator in 20 parts of deionized water to prepare an initiator solution; Add the remaining 160 parts of deionized water and 1 / 3 of the pre-emulsion to the reactor, stir, and purge the air with nitrogen for 15 minutes; slowly raise the temperature to 75±1℃, and add about 1 / 3 of the initiator solution to the reactor; maintain the temperature and react for about 30 minutes; at the same time, begin to add the remaining pre-emulsion (to be added dropwise at a uniform rate over 2 hours) and the remaining initiator solution (to be added dropwise at a uniform rate over 2.5 hours); after the addition is complete, raise the temperature of the reaction system to 80℃ and continue to keep the reaction at this temperature for 1 hour; Stop heating and slowly cool to below 40°C; adjust the pH of the emulsion to 5.0-6.0 with dilute acetic acid solution to obtain POSS-based acrylate emulsion.

[0023] The cotton fabric specification is: 20 s ×20 s / 108×56, twill.

[0024] Flame retardant properties of cotton fabric in the example: damaged char length 113mm, afterflame time 0s, smoldering time 0s.

[0025] UV protection performance: UPF value > 50 The flame retardant performance was tested in accordance with GB / T 5455-2014 "Determination of vertical damage length, smoldering and afterflame time of textiles".

[0026] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics, comprising the following steps: (1) Pretreatment of cotton fabrics before cold pad-batch processing; (2) Staining; (3) Finishing of functional coating paste; The functional coating paste is composed of POSS-based acrylate emulsion, thickener, and water.

2. The short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics according to claim 1, characterized in that: The pretreatment of cotton fabrics before cold pad-batch processing is specifically as follows: padding with working solution → rolling and wrapping → stacking → washing with hot water at 95℃ → drying.

3. The short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics according to claim 2, characterized in that: The working solution, by weight / volume, contains 12 g / L hydrogen peroxide, 40 g / L caustic soda, 9 g / L oxygen bleaching stabilizer, 16 g / L refining agent, 2 g / L chelating agent, 2 g / L penetrant, and the remainder is water.

4. The short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics according to claim 1, characterized in that: The POSS-based acrylate emulsion is prepared by emulsion polymerization of OvPOSS, phosphorus nitrogen-based acrylate flame retardant monomers, 2-hydroxy-4-methacryloyloxybenzophenone, butyl acrylate, styrene, methyl methacrylate, emulsifier, initiator, and water.

5. The short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics according to claim 1, characterized in that: The POSS-based acrylate emulsion is prepared by the following method: Add 200 parts deionized water, 8 parts OvPOSS, 16 parts phosphorus nitrogen acrylate flame retardant monomer, 5 parts 2-hydroxy-4-methacryloyloxybenzophenone, 60 parts butyl acrylate, 10 parts styrene, 18 parts methyl methacrylate, 3 parts cetyltrimethylammonium bromide, and 5 parts nonylphenol polyoxyethylene ether to an emulsifier, and emulsify at high speed for 30 minutes to obtain a pre-emulsion; Dissolve 1.3 parts of azobisisobutyramidine hydrochloride initiator in 20 parts of deionized water to prepare an initiator solution; Add the remaining 160 parts of deionized water and 1 / 3 of the pre-emulsion to the reactor, stir, and purge the air with nitrogen for 15 minutes; slowly raise the temperature to 75±1℃, and add about 1 / 3 of the initiator solution to the reactor; maintain the temperature and react for about 30 minutes; at the same time, start adding the remaining pre-emulsion and the remaining initiator solution dropwise; after the dropwise addition is complete, raise the temperature of the reaction system to 80℃ and continue to keep the reaction at this temperature for 1 hour; Stop heating and slowly cool to below 40°C; adjust the pH of the emulsion to 5.0-6.0 with dilute acetic acid solution to obtain POSS-based acrylate emulsion.

6. The short-process dyeing and finishing process for UV-resistant and flame-retardant cotton fabrics according to claim 1, characterized in that: The thickener is a nonionic thickener.

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