A fabric darkening agent and its preparation method and application

Abstract

The present application relates to the field of fabric dyeing and finishing technology, and specifically discloses a kind of fabric deepening agent and its preparation method and application. Fabric deepening agent, including the following raw materials in parts by weight: 20 40 parts of fluorinated amino silicone oil, 10 25 parts of nano silicon dioxide dispersion, 2 6 parts of emulsifier, 60 100 parts of water;And fluorinated amino silicone oil, including the following raw materials in parts by weight: 40 80 parts of terminal hydroxyl silicone oil, 20 40 parts of fluorinated amino coupling agent, 0.1 1 parts of alkaline catalyst;The preparation method of fabric deepening agent is to first add emulsifier into water, stir and mix 0.5 1min, then add nano silicon dioxide dispersion, continue stirring 1 2h, finally add fluorinated amino silicone oil, after homogenizing 20 50min, adjust pH to neutral and obtain;Above-mentioned steps are simple, and cost is low, and gained fabric deepening agent can provide the construction and low refractive index of rough surface, and the two synergistically realize the deepening of dyed fabric, and can significantly improve the color fastness of dyed fabric, with broad market prospects.

Description

Technical Field

[0001] The present application relates to the technical field of fabric dyeing and finishing, and more specifically, to a fabric darkening agent and a preparation method and application thereof. Background Art

[0002] Polyester fiber is widely favored by consumers due to its excellent physical, mechanical, and wearability properties. It has become the fastest-growing and highest-volume synthetic fiber. However, in the field of polyester fiber dyeing, due to its fine fiber size, high crystallinity, smooth surface, high refractive index, large specific surface area, and almost no reactive groups, it is difficult to dye polyester fibers in dark colors, thus limiting its wider development.

[0003] Currently, existing darkening agents achieve a desired darkening effect by coating the surface of polyester fabric with one or more layers of low-refractive-index film, altering the fiber's light reflection and refraction. Commonly used film-forming substances include organic fluorine, organic silicone, and acrylate resins. While these materials offer distinct darkening effects, they struggle to balance colorfastness and color shade. This often results in a significant decrease in the dry friction grade of the fabric and significant staining, impacting fabric performance. Therefore, there is an urgent need to address this dilemma of achieving both darkening and colorfastness for polyester fibers in order to produce high-quality polyester textiles. Summary of the Invention

[0004] In order to solve the problem that existing polyester fibers cannot achieve both darkening effect and color fastness, the present application provides a fabric darkening agent and a preparation method and application thereof.

[0005] In the first aspect, the present application provides a fabric darkening agent, which adopts the following technical solution:

[0006] A fabric darkening agent comprises the following raw materials in parts by weight: 20-40 parts of fluorinated amino silicone oil, 10-25 parts of nano-silicon dioxide dispersion, 2-6 parts of emulsifier, and 60-100 parts of water;

[0007] The fluorinated amino silicone oil comprises the following raw materials in parts by weight: 40-80 parts of terminal hydroxyl silicone oil, 20-40 parts of fluorinated amino coupling agent, and 0.1-1 part of alkaline catalyst.

[0008] By adopting the above-mentioned technical scheme, the fabric darkening agent of the present application uses fluorinated amino silicone oil, nano-silica dispersion, emulsifier and water as raw materials, and controls the weight of each raw material. The raw materials interact with each other, so that the fabric darkening agent not only has an excellent darkening effect, but also can effectively improve the color fastness of polyester fabrics.

[0009] Preferably, the fluorinated amino silicone oil is prepared by the following method:

[0010] The terminal hydroxyl silicone oil and the alkaline catalyst are prepolymerized at 70-80°C for 1-4 hours, and then a fluorinated amino coupling agent is added for modification. The reaction is carried out in vacuum for 4-8 hours. After the reaction is completed, the pH is adjusted to neutral, and the temperature is raised to 100-110°C and heated for 20-40 minutes, and then cooled to room temperature to obtain the fluorinated amino silicone oil.

[0011] By adopting the above-mentioned technical scheme, the present application uses terminal hydroxyl silicone oil and fluorinated amino coupling agent as raw materials, and introduces fluorine-containing and amino-containing groups into the silicone oil molecular chain under the action of an alkaline catalyst. Since the surface energy of fluorine is very small, it can spontaneously cover other functional groups, and the amino-containing group has a strong affinity with the fabric. Therefore, the fluorinated amino silicone oil has a lower refractive index, and then after the polyester fabric is treated with the fabric darkening agent, the apparent refractive index of the polyester fiber is reduced, which can reduce the amount of reflected light and increase the specific gravity of absorbed light, thereby increasing the apparent dyeing depth, and the darkening effect of the polyester fabric is more obvious; at the same time, a chemical bonding reaction can occur between the fluorinated amino silicone oil and the polyester fiber, the cross-linking effect is increased, and a thin film with excellent mechanical properties is formed on the surface of the polyester fiber, which increases the color fastness of the polyester fabric.

[0012] Preferably, the fluorinated amino coupling agent is prepared by the following method:

[0013] At 60-65° C., add an aminosilane coupling agent to a solvent, add trifluoropropyltrimethoxysilane, and react for 2-3 hours to obtain a fluorinated amino coupling agent.

[0014] Preferably, the aminosilane coupling agent is obtained by compounding 3-aminopropyltriethoxysilane and N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane in a mass ratio of 2:1-5.

[0015] Preferably, the mass ratio of the aminosilane coupling agent, the solvent, and trifluoropropyltrimethoxysilane is 5-8:10-15:1.

[0016] Preferably, the solvent is at least one of ethanol, tetrahydrofuran and acetonitrile.

[0017] By adopting the above technical solution, the aminosilane coupling agent of the present application is obtained by compounding 3-aminopropyltriethoxysilane and N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane. The two work synergistically to increase the active groups of the fluorinated amino coupling agent, so that the fluorinated amino coupling agent can better react with the terminal hydroxyl silicone oil, increase the cross-linking density, and thereby increase the complexity of the microstructure of the surface film covering the polyester fiber, thereby significantly improving the darkening effect of the fabric darkening agent.

[0018] Preferably, the terminal hydroxyl silicone oil is one of terminal hydroxymethyl silicone oil, terminal hydroxyethyl silicone oil and terminal hydroxypropyl silicone oil.

[0019] Preferably, the molecular weight of the hydroxy-terminated silicone oil is 500-2000.

[0020] Preferably, the alkaline catalyst is one of tetramethylammonium hydroxide, triethylamine and sodium hydroxide.

[0021] Preferably, the nano-silicon dioxide dispersion is prepared by the following method:

[0022] First, add 11-18 parts of nano-silica and 4-8 parts of cinnamic acid to 40-80 parts of water by weight, and stir and react at 60-80°C for 1-2 hours; then add 5-9 parts of sodium polystyrene sulfonate, and ultrasonically disperse for 2-3 hours to obtain a nano-silica dispersion.

[0023] By adopting the above technical solution, the present application first uses cinnamic acid to treat nano-silica, and cinnamic acid is coated on the surface of nano-silica, and then sodium polystyrene sulfonate is used for dispersion. Sodium polystyrene sulfonate has good affinity with the phenylpropenyl group of the cinnamic acid molecule. The sulfonic acid group of sodium polystyrene sulfonate has a strong wetting and dispersing effect, which can make the nano-silica particles evenly dispersed in the dispersion, reduce the agglomeration of nano-silica, and thus make the nano-silica particles evenly dispersed in the film, and can cooperate with fluorinated amino silicone oil to enhance the strength of the film and the interaction between the film and polyester fabric, effectively improving the friction fastness performance of the polyester fabric; at the same time, the addition of the nano-silica dispersion increases the roughness of the film surface, making it easy for incident light to be refracted and diffusely reflected on the surface of the polyester fiber, and reducing reflected light, thereby greatly increasing the absorption of incident light by the polyester fiber, achieving the effect of enhancing color depth.

[0024] Preferably, the emulsifier is obtained by compounding isomeric tridecanol polyoxyethylene ether, glucose amide and carageenan in a mass ratio of 2-4:3:1.

[0025] By adopting the above technical solution, the emulsifier of the present application is obtained by compounding isomeric tridecanol polyoxyethylene ether, glucose amide and carageenan. The three interact with each other to improve the feel and softness of polyester fabrics and enhance the texture of polyester fabrics.

[0026] In a second aspect, the present application provides a method for preparing a fabric darkening agent, which adopts the following technical solution:

[0027] A method for preparing a fabric darkening agent comprises the following steps:

[0028] First, add the emulsifier into water and stir for 0.5-1min, then add the nano-silicon dioxide dispersion and continue stirring for 1-2h, and finally add the fluorinated amino silicone oil, homogenize for 20-50min, and adjust the pH to neutral to obtain the fabric darkening agent.

[0029] By adopting the above technical scheme, during the preparation process of the fabric darkening agent, various process parameters are controlled, the interaction between the raw materials is promoted, and the darkening function of the fabric darkening agent is improved. The preparation method of the fabric darkening agent of the present application has simple steps, low cost, and is suitable for industrial production.

[0030] In a third aspect, the present application provides an application of a fabric darkening agent, which adopts the following technical solution:

[0031] The invention discloses an application of a fabric darkening agent, wherein the prepared fabric darkening agent is used in the post-finishing process of dyed polyester fabric.

[0032] Preferably, the post-finishing process of the dyed polyester fabric comprises the following steps:

[0033] S1. Mixing the fabric darkening agent with water in a mass ratio of 11-20:100 to obtain darkening finishing liquid A; mixing the fabric darkening agent with water in a mass ratio of 2-9:100 to obtain darkening finishing liquid B;

[0034] S2. Darkening the dyed polyester fabric by padding. First, use darkening finishing liquid A, the padding temperature is 70-80°C, the padding speed is 40-50m / min, the padding liquid rate is 60-70%, and after taking out, it is dried at 150-160°C for 5-8min; then use darkening finishing liquid B, the padding temperature is 70-80°C, the padding speed is 60-70m / min, the padding liquid rate is 40-50%, and after taking out, it is dried at 170-180°C for 5-8min to complete the darkening of the polyester fabric.

[0035] By adopting the above technical solution, the fabric darkening agent of the present application can be widely used in the finishing process of dyed polyester fabrics. The method of use is simple, and while effectively darkening the fabric, it can also improve the color fastness of the fabric.

[0036] In summary, this application has the following beneficial effects:

[0037] 1. The fabric darkening agent of the present application uses a fluorinated amino coupling agent, a nano-silica dispersion, an emulsifier and water as main raw materials. The obtained fabric darkening agent can provide rough surface construction and a low refractive index, and the two work synergistically to achieve darkening of dyed fabrics.

[0038] 2. The preparation method of the fabric darkening agent of the present application has simple steps, low cost and low equipment requirements; the obtained fabric darkening agent is used in the finishing process of dyed polyester fabrics, which significantly improves the darkening rate and color fastness of the polyester fabric, achieving the purpose of both good darkening effect and high color fastness, and has broad market prospects. DETAILED DESCRIPTION

[0039] The present application is further described in detail below with reference to the embodiments.

[0040] Preparation Examples 1-5 provide methods for preparing fluorinated amino coupling agents.

[0041] Preparation Example 1

[0042] Fluorinated amino coupling agent, prepared by the following method:

[0043] At 60°C, 5 kg of aminosilane coupling agent was added to 10 kg of solvent, and 1 kg of trifluoropropyltrimethoxysilane was added. The mixture was reacted at a speed of 300 r / min for 2 h to obtain a fluorinated amino coupling agent.

[0044] The aminosilane coupling agent is prepared by compounding 3-aminopropyltriethoxysilane and N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane in a mass ratio of 2:1; and the solvent is tetrahydrofuran.

[0045] Preparation Example 2

[0046] Fluorinated amino coupling agent, prepared by the following method:

[0047] At 63°C, 6 kg of aminosilane coupling agent was added to 13 kg of solvent, and 1 kg of trifluoropropyltrimethoxysilane was added. The mixture was reacted at a speed of 450 r / min for 2.5 h to obtain a fluorinated amino coupling agent.

[0048] The aminosilane coupling agent is prepared by compounding 3-aminopropyltriethoxysilane and N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane in a mass ratio of 2:3; and the solvent is ethanol.

[0049] Preparation Example 3

[0050] Fluorinated amino coupling agent, prepared by the following method:

[0051] At 65°C, 8 kg of aminosilane coupling agent was added to 15 kg of solvent, and 1 kg of trifluoropropyltrimethoxysilane was added. The mixture was reacted at a speed of 600 r / min for 3 h to obtain a fluorinated amino coupling agent.

[0052] The aminosilane coupling agent is prepared by compounding 3-aminopropyltriethoxysilane and N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane in a mass ratio of 2:5; and the solvent is acetonitrile.

[0053] Preparation Example 4

[0054] Preparation Example 4 is different from Preparation Example 1 only in that the aminosilane coupling agent is 3-aminopropyltriethoxysilane.

[0055] Preparation Example 5

[0056] Preparation Example 5 is different from Preparation Example 1 only in that the aminosilane coupling agent is N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane.

[0057] Preparation Examples 6-10 provide fluorinated amino silicone oils and preparation methods thereof.

[0058] Preparation Example 6

[0059] Fluorinated amino silicone oil, comprising the following raw materials: 40 kg of terminal hydroxyl silicone oil, 20 kg of fluorinated amino coupling agent, and 0.1 kg of alkaline catalyst; wherein the terminal hydroxyl silicone oil is terminal hydroxymethyl silicone oil with a molecular weight of 500; the fluorinated amino coupling agent is prepared according to Preparation Example 1; and the alkaline catalyst is tetramethylammonium hydroxide;

[0060] Fluorinated amino silicone oil is prepared by the following method:

[0061] The terminal hydroxyl silicone oil and the alkaline catalyst were prepolymerized at 70°C for 1 hour, and then a fluorinated amino coupling agent was added for modification. The reaction was carried out in vacuum for 4 hours. After the reaction was completed, the pH was adjusted to neutral, and the temperature was raised to 100°C and heated for 20 minutes, and then cooled to room temperature to obtain fluorinated amino silicone oil.

[0062] Preparation Example 7

[0063] Fluorinated amino silicone oil, comprising the following raw materials: 60 kg of hydroxyl-terminated silicone oil, 30 kg of fluorinated amino coupling agent, and 0.5 kg of alkaline catalyst; wherein the hydroxyl-terminated silicone oil is hydroxyethyl-terminated silicone oil with a molecular weight of 1000; the fluorinated amino coupling agent is prepared according to Preparation Example 2; and the alkaline catalyst is triethylamine;

[0064] Fluorinated amino silicone oil is prepared by the following method:

[0065] The terminal hydroxyl silicone oil and the alkaline catalyst were prepolymerized at 75°C for 2 hours, and then a fluorinated amino coupling agent was added for modification. The reaction was carried out in vacuum for 6 hours. After the reaction was completed, the pH was adjusted to neutral, and the temperature was raised to 105°C and heated for 30 minutes, and then cooled to room temperature to obtain fluorinated amino silicone oil.

[0066] Preparation Example 8

[0067] Fluorinated amino silicone oil, comprising the following raw materials: 80 kg of terminal hydroxyl silicone oil, 40 kg of fluorinated amino coupling agent, and 1 kg of alkaline catalyst; wherein the terminal hydroxyl silicone oil is terminal hydroxypropyl silicone oil with a molecular weight of 2000; the fluorinated amino coupling agent is prepared according to Preparation Example 3; and the alkaline catalyst is sodium hydroxide;

[0068] Fluorinated amino silicone oil is prepared by the following method:

[0069] The terminal hydroxyl silicone oil and the alkaline catalyst were prepolymerized at 80°C for 4 hours, and then a fluorinated amino coupling agent was added for modification. The reaction was carried out in vacuum for 8 hours. After the reaction was completed, the pH was adjusted to neutral, and the temperature was raised to 110°C and heated for 40 minutes, and then cooled to room temperature to obtain fluorinated amino silicone oil.

[0070] Preparation Example 9

[0071] Preparation Example 9 is different from Preparation Example 6 only in that the fluorinated amino coupling agent is prepared from Preparation Example 4.

[0072] Preparation Example 10

[0073] Preparation Example 10 is different from Preparation Example 6 only in that the fluorinated amino coupling agent is prepared from Preparation Example 5.

[0074] Comparative Preparation Examples 1 and 2 provide amino silicone oil and preparation methods thereof.

[0075] Comparative Preparation Example 1

[0076] Amino silicone oil, including the following raw materials: 40 kg of hydroxyl-terminated silicone oil, 20 kg of 3-aminopropyltriethoxysilane, and 0.1 kg of alkaline catalyst;

[0077] Wherein, the terminal hydroxyl silicone oil is a terminal hydroxymethyl silicone oil with a molecular weight of 500; the alkaline catalyst is tetramethylammonium hydroxide;

[0078] Amino silicone oil is prepared by the following method:

[0079] The terminal hydroxy silicone oil and the alkaline catalyst were prepolymerized at 70°C for 1 hour, and then 3-aminopropyltriethoxysilane was added for modification. The reaction was carried out in vacuum for 4 hours. After the reaction was completed, the pH was adjusted to neutral, and the temperature was raised to 100°C and heated for 20 minutes, and then cooled to room temperature to obtain amino silicone oil.

[0080] Comparative Preparation Example 2

[0081] Amino silicone oil, including the following raw materials: 40 kg of hydroxy-terminated silicone oil, 20 kg of N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane, and 0.1 kg of alkaline catalyst;

[0082] Wherein, the terminal hydroxyl silicone oil is a terminal hydroxymethyl silicone oil with a molecular weight of 500; the alkaline catalyst is tetramethylammonium hydroxide;

[0083] Amino silicone oil is prepared by the following method:

[0084] The terminal hydroxy silicone oil and the alkaline catalyst were prepolymerized at 70°C for 1 hour, and then N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane was added for modification. The reaction was carried out in vacuum for 4 hours. After the reaction was completed, the pH was adjusted to neutral, and the temperature was raised to 100°C and heated for 20 minutes, and then cooled to room temperature to obtain amino silicone oil.

[0085] Comparative Preparation Example 3 provides fluorinated silicone oil and a preparation method thereof.

[0086] Comparative Preparation Example 3

[0087] Fluorinated silicone oil, including the following raw materials: 40 kg of hydroxyl-terminated silicone oil, 20 kg of trifluoropropyltrimethoxysilane, and 0.1 kg of alkaline catalyst;

[0088] Wherein, the terminal hydroxyl silicone oil is a terminal hydroxymethyl silicone oil with a molecular weight of 500; the alkaline catalyst is tetramethylammonium hydroxide;

[0089] Fluorinated silicone oil is prepared by the following method:

[0090] The terminal hydroxyl silicone oil and the alkaline catalyst were prepolymerized at 70°C for 1 hour, and then trifluoropropyltrimethoxysilane was added for modification. The reaction was carried out in vacuum for 4 hours. After the reaction was completed, the pH was adjusted to neutral, and the temperature was raised to 100°C and heated for 20 minutes, and then cooled to room temperature to obtain fluorinated silicone oil.

[0091] Preparation Examples 11-15 provide methods for preparing nano-silicon dioxide dispersions.

[0092] Preparation Example 11

[0093] Nano-silicon dioxide dispersion is prepared by the following method:

[0094] First, 11 kg of nano-silica and 4 kg of cinnamic acid were added to 40 kg of water, stirred at 60 ° C and a speed of 400 r / min for 1 hour; then 5 kg of sodium polystyrene sulfonate was added, and ultrasonic dispersion was carried out at an ultrasonic power of 10 kW and an ultrasonic frequency of 20 kHz for 2 hours to obtain a nano-silica dispersion.

[0095] Preparation Example 12

[0096] Nano-silicon dioxide dispersion is prepared by the following method:

[0097] First, 15 kg of nano-silica and 6 kg of cinnamic acid were added to 60 kg of water, stirred at 70 ° C and a speed of 600 r / min for 1.5 hours; then 7 kg of sodium polystyrene sulfonate was added, and ultrasonic dispersion was carried out at an ultrasonic power of 50 kW and an ultrasonic frequency of 25 kHz for 2.5 hours to obtain a nano-silica dispersion.

[0098] Preparation Example 13

[0099] Nano-silicon dioxide dispersion is prepared by the following method:

[0100] First, 18 kg of nano-silica and 8 kg of cinnamic acid were added to 80 kg of water, stirred at 80 ° C and a speed of 800 r / min for 2 hours; then 9 kg of sodium polystyrene sulfonate was added, and ultrasonic dispersion was carried out at an ultrasonic power of 100 kW and an ultrasonic frequency of 30 kHz for 3 hours to obtain a nano-silica dispersion.

[0101] Preparation Example 14

[0102] Preparation Example 14 is the same as Preparation Example 11 except that an equal amount of citric acid is used to replace cinnamic acid.

[0103] Preparation Example 15

[0104] Preparation Example 15 is the same as Preparation Example 11 except that an equal mass of sodium lignin sulfonate is used to replace sodium polystyrene sulfonate.

[0105] Examples 1-10 provide a fabric darkening agent and a preparation method thereof.

[0106] Example 1

[0107] Fabric darkening agent, including the following raw materials: 40kg fluorinated amino silicone oil, 25kg nano-silicon dioxide dispersion, 6kg emulsifier, 100kg water;

[0108] Among them, the fluorinated amino silicone oil was prepared by Preparation Example 6; the nano-silicon dioxide dispersion was prepared by Preparation Example 11; and the emulsifier was prepared by compounding isomeric tridecanol polyoxyethylene ether, glucosamide, and carrageenan in a mass ratio of 2:3:1;

[0109] The preparation method of the fabric darkening agent comprises the following steps:

[0110] First, add the emulsifier into the water and stir at a speed of 400 r / min for 0.5 min. Then add the nano-silica dispersion and continue stirring at a speed of 1000 r / min for 1 h. Finally, add the fluorinated amino silicone oil and homogenize at a speed of 4000 rpm and a homogenization pressure of 800 bar for 20 min. Then, adjust the pH to neutral to obtain the fabric darkening agent.

[0111] Example 2

[0112] Fabric darkening agent, including the following raw materials: 30kg of fluorinated amino silicone oil, 15kg of nano-silica dispersion, 4kg of emulsifier, and 80kg of water;

[0113] Among them, the fluorinated amino silicone oil was prepared by Preparation Example 8; the nano-silicon dioxide dispersion was prepared by Preparation Example 12; and the emulsifier was prepared by compounding isomeric tridecanol polyoxyethylene ether, glucosamide, and carrageenan in a mass ratio of 3:3:1;

[0114] The preparation method of the fabric darkening agent comprises the following steps:

[0115] First, add the emulsifier into the water and stir at a speed of 500 r / min for 0.8 min. Then add the nano-silica dispersion and continue stirring at a speed of 1500 r / min for 1.5 h. Finally, add the fluorinated amino silicone oil and homogenize at a speed of 7000 rpm and a homogenization pressure of 900 bar for 35 min. Then, adjust the pH to neutral to obtain the fabric darkening agent.

[0116] Example 3

[0117] Fabric darkening agent, including the following raw materials: 40kg fluorinated amino silicone oil, 25kg nano-silicon dioxide dispersion, 6kg emulsifier, 100kg water;

[0118] Among them, the fluorinated amino silicone oil was prepared by Preparation Example 8; the nano-silicon dioxide dispersion was prepared by Preparation Example 13; and the emulsifier was prepared by compounding isomeric tridecanol polyoxyethylene ether, glucosamide, and carrageenan in a mass ratio of 4:3:1;

[0119] The preparation method of the fabric darkening agent comprises the following steps:

[0120] First, add the emulsifier into the water and stir at a speed of 600 r / min for 1 minute. Then add the nano-silica dispersion and continue stirring at a speed of 2000 r / min for 2 hours. Finally, add the fluorinated amino silicone oil and homogenize at a speed of 10000 rpm and a homogenization pressure of 1000 bar for 50 minutes. Then, adjust the pH to neutral to obtain the fabric darkening agent.

[0121] Example 4

[0122] Example 4 is different from Example 1 only in that the fluorinated amino silicone oil is prepared by Preparation Example 9.

[0123] Example 5

[0124] Example 5 is different from Example 1 only in that the fluorinated amino silicone oil is prepared by Preparation Example 10.

[0125] Example 6

[0126] Example 6 is different from Example 1 only in that the nano-silica dispersion is prepared by Preparation Example 14.

[0127] Example 7

[0128] Example 7 is different from Example 1 only in that the nano-silica dispersion is prepared by Preparation Example 15.

[0129] Example 8

[0130] Example 8 is different from Example 1 only in that the emulsifier is obtained by compounding isomeric tridecanol polyoxyethylene ether and glucose amide in a mass ratio of 2:3.

[0131] Example 9

[0132] Example 9 is different from Example 1 only in that the emulsifier is obtained by compounding isomeric tridecanol polyoxyethylene ether and carageenan in a mass ratio of 2:1.

[0133] Example 10

[0134] Example 10 is different from Example 1 only in that the emulsifier is obtained by compounding glucosamide and carageenan in a mass ratio of 3:1.

[0135] In order to verify the performance of the fabric darkening agent in Examples 1-10 of the present application, the applicant set up comparative examples 1-7, which are as follows:

[0136] Comparative Example 1

[0137] Comparative Example 1 is different from Example 1 only in that an equal mass of amino silicone oil is used to replace the fluorinated amino silicone oil, and the amino silicone oil is prepared by Comparative Preparation Example 1.

[0138] Comparative Example 2

[0139] Comparative Example 2 is different from Example 1 only in that an equal mass of amino silicone oil is used to replace the fluorinated amino silicone oil, and the amino silicone oil is prepared by Comparative Preparation Example 2.

[0140] Comparative Example 3

[0141] Comparative Example 3 is different from Example 1 only in that an equal mass of fluorinated silicone oil is used to replace the fluorinated amino silicone oil, and the fluorinated silicone oil is prepared by Comparative Preparation Example 3.

[0142] Comparative Example 4

[0143] Comparative Example 4 is different from Example 1 only in that an equal mass of nano-silica is used to replace the nano-silica dispersion.

[0144] Comparative Example 5

[0145] Comparative Example 5 is the same as Example 1 except that an equal amount of fluorinated amino silicone oil is used to replace the nano-silica dispersion.

[0146] Comparative Example 6

[0147] Comparative Example 6 is the same as Example 1 except that an equal mass of nano-silica dispersion is used to replace the fluorinated amino silicone oil.

[0148] Comparative Example 7

[0149] Comparative Example 7 is different from Example 1 only in that no emulsifier is added.

[0150] Application Examples 1-10 and Comparative Application Examples 1-7 provide fabric darkening agents for use in the post-finishing process of dyed polyester fabrics.

[0151] Application Example 1

[0152] The finishing process of dyed polyester fabric includes the following steps:

[0153] S1. Mix 11 kg of fabric darkening agent with 100 kg of water to obtain darkening finishing liquid A; mix 2 kg of fabric darkening agent with 100 kg of water to obtain darkening finishing liquid B;

[0154] Wherein, the fabric darkening agent is prepared by Example 1;

[0155] S2. The black polyester fabric is darkened by padding. First, darkening finishing liquid A is used, the padding temperature is 70°C, the padding speed is 40m / min, the padding liquid rate is 60%, and after taking out, it is dried at 150°C for 5 minutes; then darkening finishing liquid B is used, the padding temperature is 70°C, the padding speed is 60m / min, the padding liquid rate is 40%, and after taking out, it is dried at 170°C for 5 minutes to complete the darkening of the polyester fabric.

[0156] Application Example 2

[0157] The finishing process of dyed polyester fabric includes the following steps:

[0158] S1. Mix 15 kg of fabric darkening agent with 100 kg of water to obtain darkening finishing liquid A; mix 6 kg of fabric darkening agent with 100 kg of water to obtain darkening finishing liquid B;

[0159] Wherein, the fabric darkening agent is prepared by Example 2;

[0160] S2. The black polyester fabric was darkened by padding. First, darkening finishing liquid A was used, the padding temperature was 75°C, the padding speed was 45m / min, the padding liquid rate was 65%, and after taking out, it was dried at 155°C for 7min; then darkening finishing liquid B was used, the padding temperature was 75°C, the padding speed was 65m / min, the padding liquid rate was 45%, and after taking out, it was dried at 175°C for 7min to complete the darkening of the polyester fabric.

[0161] Application Example 3

[0162] The finishing process of dyed polyester fabric includes the following steps:

[0163] S1. Mix 20 kg of fabric darkening agent with 100 kg of water to obtain darkening finishing liquid A; mix 9 kg of fabric darkening agent with 100 kg of water to obtain darkening finishing liquid B;

[0164] Wherein, the fabric darkening agent is prepared by Example 3;

[0165] S2. The black polyester fabric was darkened by padding. First, darkening finishing liquid A was used, the padding temperature was 80°C, the padding speed was 50m / min, the padding liquid rate was 70%, and after taking out, it was dried at 160°C for 8 minutes; then darkening finishing liquid B was used, the padding temperature was 80°C, the padding speed was 70m / min, the padding liquid rate was 50%, and after taking out, it was dried at 180°C for 8 minutes to complete the darkening of the polyester fabric.

[0166] Application Example 4-10

[0167] Application Examples 4-10 are different from Application Example 1 only in that the fabric darkening agents are prepared from Examples 4-10 respectively.

[0168] Comparative Application Examples 1-7

[0169] Comparative Application Examples 1-7 are different from Application Example 1 only in that the fabric darkening agents are prepared from Comparative Examples 1-7 respectively.

[0170] The darkening effects of the dyed polyester fabrics in Application Examples 1-10 of the present application and Comparative Application Examples 1-7 were tested respectively, and the following result parameters were obtained, as shown in Table 1:

[0171] K / S value and darkening rate: The base fabric is tested using a Datacolor colorimeter. The K / S value of the standard dyeing depth is used as the evaluation standard. The darkening rate is calculated using the following formula:

[0172] Deepening rate = [(K / S)2-(K / S)1] / (K / S)1×100%, where: (K / S)1 represents the K / S value of the undeepened base fabric, and (K / S)2 represents the K / S value of the deepened base fabric;

[0173] Color fastness to rubbing and color fastness to washing with soap test: According to GB / T 3920-2008 "Textiles — Tests for color fastness — Color fastness to rubbing", the color fastness to rubbing of the samples was tested using a manual rubbing fastness meter; according to GB / T 3921-2008 "Textiles — Tests for color fastness — Color fastness to washing with soap", the color fastness to washing with soap tester was tested.

[0174] Table 1:

[0175]

[0176] It can be seen from the data shown in Table 1 above that the darkening effect of the dyed polyester fabric in Application Examples 1-10 of the present application is far better than the darkening effect in Comparative Application Examples 1-7, with a large K / S value, bright colors, a high darkening rate, and excellent color fastness to friction and color fastness to soaping. The fabric darkening agent of the present application achieves the purpose of achieving a balance between darkening effect and color fastness.

[0177] It can be seen from Application Example 1 and Application Examples 4 and 5 that the fabric darkening agent used in Application Example 1 is prepared by Example 1, and Example 1 uses the fluorinated amino silicone oil prepared in Preparation Example 6 as a raw material, and the fluorinated amino silicone oil uses the fluorinated amino coupling agent prepared in Preparation Example 1 as a raw material. Compared with Application Examples 4 and 5, the darkening effect of Application Example 1 is more obvious, and the color fastness of the dyed polyester fabric is higher, indicating that 3-aminopropyltriethoxysilane and N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane have a synergistic effect, which makes the performance of the darkening agent more excellent.

[0178] It can be seen from Application Examples 1 and Application Examples 6 and 7 that the fabric darkening agent used in Application Example 1 is prepared by Example 1. Example 1 uses the nano-silica dispersion prepared in Preparation Example 11 as a raw material. In Preparation Example 11, the nano-silica is first treated with cinnamic acid, and then the nano-silica is dispersed with sodium polyethylene benzene sulfonate. Compared with Application Examples 6 and 7, the dyed polyester fabric in Application Example 1 is effectively darkened, and the color fastness to rubbing and the color fastness to soaping are also significantly improved.

[0179] It can be seen from Application Example 1 and Application Examples 8-10 that the fabric darkening agent used in Application Example 1 is prepared by Example 1, and the emulsifier in Example 1 is obtained by compounding isomeric tridecanol polyoxyethylene ether, glucose amide and carageenan. Compared with Application Examples 8-10, the darkening rate of the dyed polyester fabric in Application Example 1 is higher, the darkening effect is more excellent, and the color fastness of the fabric is greatly improved.

[0180] It can be seen from Application Example 1 and Comparative Application Examples 1-3 that the fabric darkening agent used in Application Example 1 is prepared by Example 1, and Example 1 uses the fluorinated amino silicone oil prepared in Preparation Example 6 as raw material. Compared with Comparative Application Examples 1-3, the darkening effect of the dyed polyester fabric in Application Example 1 is improved, and the color fastness of the fabric is also significantly improved.

[0181] It can be seen from Application Example 1 and Application Comparative Example 4 that the fabric darkening agent used in Application Example 1 is prepared by Example 1, and Example 1 uses the nano-silicon dioxide dispersion prepared in Preparation Example 11 as raw material. Compared with Application Comparative Example 4, the color fastness of the dyed polyester fabric in Application Example 1 is improved.

[0182] It can be seen from Application Example 1 and Application Comparative Examples 5 and 6 that the fabric darkening agent used in Application Example 1 is prepared from Example 1, and Example 1 uses fluorinated amino silicone oil and nano-silicon dioxide dispersion as raw materials. Compared with Application Comparative Examples 5 and 6, the polyester fabric of Application Example 1 is brighter in color and has a more obvious darkening effect.

[0183] It can be seen from Application Example 1 and Application Comparative Example 7 that the fabric darkening agent used in Application Example 1 is prepared from Example 1, and an emulsifier is added to the raw materials of Example 1. Compared with Application Comparative Example 7, the color fastness of the polyester fabric in Application Example 1 is higher and the color is brighter.

[0184] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A fabric darkening agent, characterized in that: The method comprises the following raw materials in parts by weight: 20-40 parts of fluorinated amino silicone oil, 10-25 parts of nano-silicon dioxide dispersion, 2-6 parts of emulsifier, and 60-100 parts of water; The fluorinated amino silicone oil comprises the following raw materials in parts by weight: 40-80 parts of terminal hydroxyl silicone oil, 20-40 parts of fluorinated amino coupling agent, and 0.1-1 part of alkaline catalyst; The fluorinated amino coupling agent is prepared by the following method: At 60-65° C., an aminosilane coupling agent is added to a solvent, and trifluoropropyltrimethoxysilane is added, and the reaction is carried out for 2-3 hours to obtain a fluorinated amino coupling agent; wherein the aminosilane coupling agent is obtained by compounding 3-aminopropyltriethoxysilane and N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane in a mass ratio of 2:1-5; The nano-silicon dioxide dispersion is prepared by the following method: First, add 11-18 parts of nano-silica and 4-8 parts of cinnamic acid to 40-80 parts of water by weight, and stir at 60-80°C for 1-2 hours; then add 5-9 parts of sodium polystyrene sulfonate, and ultrasonically disperse for 2-3 hours to obtain a nano-silica dispersion; The emulsifier is prepared by compounding isomeric tridecanol polyoxyethylene ether, glucose amide and carageenan in a mass ratio of 2-4:3:

1.

2. The fabric darkening agent according to claim 1, characterized in that The fluorinated amino silicone oil is prepared by the following method: The terminal hydroxyl silicone oil and the alkaline catalyst are prepolymerized at 70-80°C for 1-4 hours, and then a fluorinated amino coupling agent is added for modification. The reaction is carried out in vacuum for 4-8 hours. After the reaction is completed, the pH is adjusted to neutral, and the temperature is raised to 100-110°C and heated for 20-40 minutes, and then cooled to room temperature to obtain the fluorinated amino silicone oil.

3. The fabric darkening agent according to claim 1, characterized in that The mass ratio of the aminosilane coupling agent, the solvent and trifluoropropyltrimethoxysilane is 5-8:10-15:

1.

4. A method for preparing the fabric darkening agent according to any one of claims 1 to 3, characterized in that: The following steps are involved: First, add the emulsifier into water and stir for 0.5-1min, then add the nano-silicon dioxide dispersion and continue stirring for 1-2h, and finally add the fluorinated amino silicone oil, homogenize for 20-50min, and adjust the pH to neutral to obtain the fabric darkening agent.

5. A use of the fabric darkening agent according to any one of claims 1 to 3, characterized in that: The prepared fabric darkening agent is used in the post-finishing process of dyed polyester fabrics.

6. The use according to claim 5, characterized in that The post-finishing process of the dyed polyester fabric comprises the following steps: S1. Mixing the fabric darkening agent with water in a mass ratio of 11-20:100 to obtain darkening finishing liquid A; mixing the fabric darkening agent with water in a mass ratio of 2-9:100 to obtain darkening finishing liquid B; S2. Darkening the dyed polyester fabric by padding. First, use darkening finishing liquid A, the padding temperature is 70-80°C, the padding speed is 40-50m / min, the padding liquid rate is 60-70%, and after taking out, it is dried at 150-160°C for 5-8min; then use darkening finishing liquid B, the padding temperature is 70-80°C, the padding speed is 60-70m / min, the padding liquid rate is 40-50%, and after taking out, it is dried at 170-180°C for 5-8min to complete the darkening of the polyester fabric.

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