Two-component resist and method of making and using same

Abstract

The application belongs to the technical field of resist materials, and particularly relates to a two-component resist, a preparation method and application thereof. The two-component resist comprises component A and component B. The two-component resist provided by the application is used as a bottom material, can protect the fabric from being left on the fabric by polyester in the component B, and can firmly graft the component B to form a hydrophilic barrier layer on the fiber surface.

Description

Technical Field

[0001] This invention belongs to the field of anti-dyeing agent materials technology, specifically relating to a two-component anti-dyeing agent, its preparation method, and its application. Background Technology

[0002] Polyester anti-dyeing agent is a key auxiliary agent used in textile printing and dyeing to prevent dyes from "blending" between different fibers. It captures free dyes through physical adsorption or chemical binding, effectively preventing "floating color" staining and thus ensuring clear patterns.

[0003] However, existing polyester anti-dyeing powders are difficult to dissolve in cold water and cannot exert their effect quickly enough to achieve the desired anti-dyeing effect. Removal usually requires heating the water to a high temperature of 70℃~90℃ and using high-speed agitation. Washing at room temperature leaves residue on the fabric, causing problems such as fabric stiffness. Summary of the Invention

[0004] To address the aforementioned problems, this invention provides a two-component anti-dyeing agent, its preparation method, and its application. This addresses at least one aspect of solving the above-mentioned technical problems.

[0005] This invention is achieved through the following technical solution: In a first aspect, the present invention provides a two-component anti-dyeing agent, comprising component A and component B; Component A includes components at the following concentrations: 150g / L~200g / L isophorone diisocyanate, 100g / L~150g / L polycaprolactone diol, 50g / L~80g / L hydroxyalkyl-terminated polysiloxane, 30g / L~50g / L N-methyldiethanolamine, 20g / L~40g / L bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 1g / L~2g / L dibutyltin dilaurate; Component B includes components at the following concentrations: 150g / L~200g / L water-soluble modified polyester, 80g / L~120g / L polyethylene glycol, 50g / L~80g / L fatty alcohol polyoxyethylene ether.

[0006] In some possible implementations, the water-soluble modified polyester is sulfonated polyethylene terephthalate, and the raw materials for preparing the sulfonated polyethylene terephthalate include a mixture of diacids and ethylene glycol.

[0007] In some possible implementations, the molar ratio of the mixed dicarboxylic acid and ethylene glycol is 1:1.2 to 1.5.

[0008] In some possible implementations, the mixed dicarboxylic acid comprises components in the following mass fractions: 85%~90% terephthalic acid, 10%~15% sodium isophthalic acid-5-sulfonate.

[0009] In some possible implementations, the raw materials for preparing the sulfonated polyethylene terephthalate also include antimony trioxide.

[0010] In some possible implementations, the amount of antimony trioxide used is 0.03% to 0.05% of the mass of terephthalic acid.

[0011] In some possible implementations, the raw materials for preparing the sulfonated polyethylene terephthalate also include triphenyl phosphate.

[0012] In some possible implementations, the mass of triphenyl phosphate is 0.01% to 0.02% of the total mass of the mixed dicarboxylic acid and ethylene glycol.

[0013] Secondly, the present invention provides a method for preparing the above-mentioned two-component anti-dyeing agent, characterized by comprising the following steps: Prepare component A and component B separately.

[0014] In some possible implementations, the preparation of component B includes the following steps: Mix water-soluble modified polyester, polyethylene glycol, fatty alcohol polyoxyethylene ether and water according to the preset concentration.

[0015] In some possible implementations, the preparation of the water-soluble modified polyester includes the following steps: The mixture of diacid, ethylene glycol and antimony trioxide was esterified and then mixed with triphenyl phosphate for polycondensation. The mixed dicarboxylic acids include terephthalic acid and sodium isophthalic acid-5-sulfonate.

[0016] In some possible implementations, the esterification treatment temperature is 220°C to 240°C.

[0017] In some possible implementations, the pressure of the esterification treatment is 0.2 MPa to 0.3 MPa.

[0018] In some possible implementations, the esterification process takes 2 to 3 hours.

[0019] In some possible implementations, the polycondensation treatment temperature is 260°C to 280°C.

[0020] In some possible implementations, the pressure of the polycondensation process is below 100 Pa.

[0021] In some possible implementations, the polycondensation process takes 1.5 h to 2.5 h.

[0022] In some possible implementations, mixing the water-soluble modified polyester, polyethylene glycol, fatty alcohol polyoxyethylene ether, and water includes the following steps: After heating water to 60℃~70℃, polyethylene glycol and water-soluble modified polyester are added to obtain a mixed system; After the mixture is cooled to 40℃~45℃, it is mixed and stirred with fatty alcohol polyoxyethylene ether.

[0023] In some possible implementations, the preparation of component A includes the following steps: Isophorone diisocyanate, polycaprolactone diol, hydroxyalkyl-terminated polysiloxane and dibutyltin dilaurate were subjected to a first mixing treatment to obtain a prepolymer; The prepolymer, N-methyldiethanolamine, and bisphenol A (2,3-dihydroxypropyl) glycidyl ether were subjected to a second mixing treatment to obtain the polymer.

[0024] In some possible implementations, the first mixing process includes the following steps: After vacuum dehydration, polycaprolactone diol is mixed with isophorone diisocyanate and dibutyltin dilaurate for catalytic reaction, and then mixed with hydroxyalkyl-terminated polysiloxane for further reaction.

[0025] In some possible implementations, the temperature of the vacuum dehydration is 115°C to 125°C.

[0026] In some possible implementations, the vacuum dehydration pressure is -0.2 MPa to -0.1 MPa.

[0027] In some possible implementations, the vacuum dehydration time is 2 to 3 hours.

[0028] In some possible implementations, the temperature of the mixed catalytic reaction is 75°C to 85°C.

[0029] In some possible implementations, the time for the mixed catalytic reaction is 2 to 3 hours.

[0030] In some possible implementations, the mixing reaction continues for 1.5 h to 2 h.

[0031] In some possible implementations, the second mixing process includes the following steps: After the prepolymer and N-methyldiethanolamine are mixed and reacted, bisphenol A (2,3-dihydroxypropyl) glycidyl ether is added and reacted.

[0032] In some possible implementations, the reaction temperature of the prepolymer and N-methyldiethanolamine is 55°C to 65°C.

[0033] In some possible implementations, the reaction time of the prepolymer and N-methyldiethanolamine is 1 h to 2 h.

[0034] In some possible implementations, the reaction time for adding bisphenol A (2,3-dihydroxypropyl) glycidyl ether is 2 to 3 hours.

[0035] Thirdly, the present invention provides a method for treating a fabric, comprising treating the fabric with the aforementioned two-component anti-dyeing agent.

[0036] The two-component anti-dyeing agent provided by this invention has at least the following beneficial technical effects compared with the prior art: The two-component anti-dyeing agent provided by this invention uses component A as a base material, which protects the fabric from polyester residue in component B, preventing problems such as fabric stiffness. Removal only requires alkaline conditions, where the quaternary ammonium cation (-NR3) of component A... + ) by OH - Neutralization transforms the component into a free amine (-NR3), the positive charge disappears, and the B component, which loses electrostatic attraction, detaches from the fiber surface and enters the aqueous phase to be washed away. It can also firmly graft the B component to form a hydrophilic barrier layer on the fiber surface, preventing dye molecules (especially disperse dyes) from contacting the fiber. At the same time, the hydration of the PEG chain segments enhances the anti-dyeing effect. Detailed Implementation

[0037] To make the objectives, technical solutions, and advantages of this invention clearer, the invention is described and illustrated below with reference to embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention. All other embodiments obtained by those skilled in the art based on the embodiments provided by this invention without inventive effort are within the scope of protection of this invention.

[0038] Obviously, the following description is merely some examples or embodiments of the present invention. Those skilled in the art can apply the present invention to other similar scenarios without any inventive effort. Furthermore, it is understood that although the effort involved in such development may be complex and lengthy, for those skilled in the art related to the content disclosed in this invention, modifications to design, manufacturing, or production based on the technical content disclosed in this invention are merely conventional technical means and should not be construed as insufficient disclosure of the present invention.

[0039] However, there may be instances where unnecessary detailed descriptions are omitted. For example, detailed descriptions of well-known matters or repetitive descriptions of essentially the same structures may be omitted. This is to avoid making the following description unnecessarily lengthy and to facilitate understanding by those skilled in the art. Furthermore, the following description is provided to enable those skilled in the art to fully understand the invention and is not intended to limit the subject matter of the claims.

[0040] Unless otherwise specified, all embodiments and optional embodiments of the present invention can be combined with each other to form new technical solutions, and all technical features and optional technical features of the present invention can be combined with each other to form new technical solutions.

[0041] Two-component anti-dyeing agent The first aspect of this invention provides a two-component anti-dyeing agent, comprising component A and component B; Component A includes components at the following concentrations: 150g / L~200g / L isophorone diisocyanate (IPDI), 100g / L~150g / L polycaprolactone diol (PCL-2000), 50g / L~80g / L hydroxyalkyl-terminated polysiloxane, 30g / L~50g / L N-methyldiethanolamine (MDEA), 20g / L~40g / L bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 1g / L~2g / L dibutyltin dilaurate; Component B includes components at the following concentrations: 150g / L~200g / L water-soluble modified polyester, 80g / L~120g / L polyethylene glycol (PEG-4000), 50g / L~80g / L fatty alcohol polyoxyethylene ether (AEO-9).

[0042] The two-component anti-dyeing agent provided in this embodiment of the invention, in component A, the tertiary amine group of N-methyldiethanolamine is protonated by acetic acid to form a quaternary ammonium cation (-NR3). + The polyurethane molecules electrostatically adsorb onto the fabric fiber surface; simultaneously, the hydroxyl and urethane groups on the polyurethane molecular chain form hydrogen bonds with the fiber, achieving a firm anchoring. In component B, the sulfonated polyester's sulfonic acid groups (-SO3)... - ) and the cationic group of component A (-NR3) + Strong ionic bonds are formed between PEG and A components. Simultaneously, the ether oxygen bonds of PEG form hydrogen bonds with the urethane groups of component A, ensuring a strong bond between component B and component A. The grafted component B forms a hydrophilic barrier layer on the fiber surface, preventing dye molecules (especially disperse dyes) from contacting the fiber. Furthermore, the hydration of the PEG segments enhances the anti-dyeing effect. During removal, under alkaline conditions, the quaternary ammonium cation (-NR3) of component A... + ) by OH -Neutralization transforms the component into a free amine (-NR3), the positive charge disappears, and the B component, which has lost its electrostatic attraction, detaches from the fiber surface and enters the aqueous phase to be washed away.

[0043] In some embodiments, the CAS number of isophorone diisocyanate is 4098-71-9.

[0044] In some embodiments, the CAS number of polycaprolactone diol is 36890-68-3.

[0045] In some specific embodiments, polycaprolactone diol is PCL-2000.

[0046] In some embodiments, the CAS number of the hydroxyl-terminated polysiloxane is 156327-07-0.

[0047] In some embodiments, the CAS number of N-methyldiethanolamine is 105-59-9.

[0048] In some embodiments, the CAS number of bisphenol A (2,3-dihydroxypropyl) glycidyl is 76002-91-0.

[0049] In some embodiments, the CAS number of dibutyltin dilaurate is 105124-36-5.

[0050] In some embodiments, the water-soluble modified polyester is sulfonated polyethylene terephthalate.

[0051] In some embodiments, the raw materials for preparing sulfonated polyethylene terephthalate include a mixture of dibasic acids and ethylene glycol.

[0052] In some embodiments, the molar ratio of the mixed dicarboxylic acid and ethylene glycol is 1:(1.2~1.5).

[0053] In some embodiments, the mixed dicarboxylic acid comprises the following components by mass fraction: 85%~90% terephthalic acid, 10%~15% sodium isophthalic acid-5-sulfonate.

[0054] In some embodiments, the raw materials for preparing sulfonated polyethylene terephthalate also include antimony trioxide. In this case, antimony trioxide acts as a catalyst to catalyze the dehydration reaction of carboxylic acids and alcohols.

[0055] In some embodiments, the amount of antimony trioxide used is 0.03% to 0.05% of the mass of terephthalic acid.

[0056] In some embodiments, the raw materials for preparing sulfonated polyethylene terephthalate also include triphenyl phosphate.

[0057] In some embodiments, the mass of triphenyl phosphate is 0.01% to 0.02% of the total mass of the mixed dicarboxylic acid and ethylene glycol.

[0058] In some embodiments, the CAS number of polyethylene glycol is 25322-68-3.

[0059] In some embodiments, the CAS number of fatty alcohol polyoxyethylene ether is 68213-23-0.

[0060] [Preparation method of two-component anti-dyeing agent] A second aspect of this invention provides a method for preparing the above-mentioned two-component anti-dyeing agent, comprising the following steps: S10. Prepare component A and component B respectively.

[0061] In some embodiments, the preparation of component A in step S10 above includes the following steps: S101. Isophorone diisocyanate, polycaprolactone diol, hydroxyalkyl-terminated polysiloxane and dibutyltin dilaurate are subjected to a first mixing treatment to obtain a prepolymer.

[0062] S102. The prepolymer, N-methyldiethanolamine and bisphenol A (2,3-dihydroxypropyl) glycidyl ether are subjected to a second mixing treatment to obtain the polymer.

[0063] In some embodiments, in step S101 above, the first mixing process includes the following steps: S1011. Polycaprolactone diol is vacuum dehydrated, then mixed with isophorone diisocyanate and dibutyltin dilaurate for catalytic reaction, and then mixed with hydroxyalkyl-terminated polysiloxane for further reaction.

[0064] In some embodiments, in step S1011 above, the temperature for vacuum dehydration is 115°C to 125°C.

[0065] In some embodiments, in step S1011 above, the pressure of vacuum dehydration is -0.2MPa to -0.1MPa.

[0066] In some embodiments, in step S1011 above, the vacuum dehydration time is 2h to 3h.

[0067] In some embodiments, in step S1011 above, the temperature of the mixed catalytic reaction is 75°C to 85°C.

[0068] In some embodiments, in step S1011 above, the time for the mixed catalytic reaction is 2h to 3h.

[0069] In some embodiments, in step S1011 above, the mixing and reaction continues for 1.5h to 2h.

[0070] In some embodiments, in step S102 above, the second mixing process includes the following steps: S1021. After the prepolymer and N-methyldiethanolamine are mixed and reacted, bisphenol A (2,3-dihydroxypropyl) glycidyl ether is added and reacted.

[0071] In some embodiments, in step S1021 above, the temperature for the reaction of the prepolymer and N-methyldiethanolamine is 55°C to 65°C.

[0072] In some embodiments, in step S1021 above, the reaction time of the prepolymer and N-methyldiethanolamine is 1h to 2h.

[0073] In some embodiments, in step S1021 above, the reaction time for adding bisphenol A (2,3-dihydroxypropyl) glycidyl ether is 2h to 3h.

[0074] In some embodiments, the preparation of component A in step S10 above further includes the following steps: S103. After mixing the polymer and glacial acetic acid, emulsification and vacuum distillation are performed.

[0075] In the preparation of component A above, the polymer and glacial acetic acid are mixed and neutralized, then emulsified, and finally distilled under reduced pressure to remove impurities from the polymer. It should be noted that mixing the polymer and glacial acetic acid, emulsification, and reduced pressure distillation are all conventional impurity removal operations in the art, and therefore are not particularly limited in this embodiment of the invention. However, as an example, the mixing time of the polymer and glacial acetic acid can be 15 minutes, the amount of glacial acetic acid can be 0.8 times the volume of the polymer, and the emulsification is performed by slowly adding deionized water under high-speed shear (2000 rpm~3000 rpm).

[0076] In some embodiments, the preparation of component A in step S10 above further includes the following steps: S104. Adjust the pH of component A to 5-6.

[0077] In some embodiments, in step S104 above, hydrochloric acid is used to adjust the pH value of component A.

[0078] In some embodiments, the preparation of component B in step S10 above includes the following steps: S105. Mix water-soluble modified polyester, polyethylene glycol, fatty alcohol polyoxyethylene ether and water according to the preset concentration.

[0079] In some embodiments, the preparation of the water-soluble modified polyester in step S105 above includes the following steps: S1051. A mixture of diacid, ethylene glycol and antimony trioxide is esterified and then mixed with triphenyl phosphate for polycondensation treatment; The mixed dicarboxylic acids include terephthalic acid and sodium isophthalic acid-5-sulfonate.

[0080] In the preparation of the above-mentioned water-soluble modified polyester, esterification treatment introduces sulfonic acid groups into the esterified molecular chain in the form of covalent bonds to generate bis(hydroxyethyl) terephthalate and its sulfonated derivatives; polycondensation polymerizes the molecules to form the modified polyester.

[0081] In some embodiments, in step S1051 above, the mixed dicarboxylic acid, ethylene glycol and antimony trioxide are mixed and esterified under an inert atmosphere.

[0082] In some embodiments, the inert atmosphere includes either a nitrogen atmosphere or an argon atmosphere.

[0083] In some embodiments, in step S1051 above, the esterification temperature is 220°C to 240°C.

[0084] In some embodiments, in step S1051 above, the pressure of the esterification treatment is 0.2 MPa to 0.3 MPa.

[0085] In some embodiments, the esterification treatment time in step S1051 is 2h to 3h.

[0086] In some embodiments, in step S1051 above, the temperature of the polycondensation treatment is 260°C to 280°C.

[0087] In some embodiments, in step S1051 described above, the pressure of the polycondensation treatment is below 100 Pa.

[0088] In some embodiments, in step S1051 above, the polycondensation treatment time is 1.5h to 2.5h.

[0089] In some embodiments, in step S105 above, mixing the water-soluble modified polyester, polyethylene glycol, fatty alcohol polyoxyethylene ether, and water includes the following steps: S1052. After heating water to 60℃~70℃, polyethylene glycol and water-soluble modified polyester are added to obtain a mixed system.

[0090] S1053. After the mixed system is cooled to 40℃~45℃, it is mixed and stirred with fatty alcohol polyoxyethylene ether.

[0091] In some embodiments, in step S1053 above, the mixing and stirring time is 30 min to 40 min.

[0092] In some embodiments, the preparation of component B in step S10 above further includes the following steps: S106. Adjust the pH of component B to 6.5~7.5.

[0093] In some embodiments, in step S106 above, the pH value of component B is adjusted using sodium hydroxide solution.

[0094] Fabric treatment methods A third aspect of the present invention provides a method for treating a fabric, comprising treating the fabric with the aforementioned two-component anti-dyeing agent.

[0095] In some embodiments, the fabric includes one of denim, corduroy, khaki, and canvas.

[0096] In some embodiments, treating the fabric with a two-component resist agent includes the following steps: s10. The fabric is treated with component A for anchoring and then with component B for grafting.

[0097] In the above two-component anti-dyeing agent treatment of fabrics, the anchoring treatment of component A causes component A to cross-link and cure on the fiber surface of the fabric; the grafting treatment of component B is that component B is grafted onto component A through ionic bonds.

[0098] In some embodiments, in step s10 above, the anchoring process for component A includes the following steps: s101. Component A is diluted with water to obtain diluted solution A.

[0099] s102. After padding the fabric with diluted solution A, pre-dry and then bake.

[0100] In some embodiments, in step s101 above, the solid content of diluent A is 5% to 10%.

[0101] In some embodiments, the pH value of diluent A in step s101 above is 5-6. It should be noted that the pH value of diluent A can be adjusted using dilute hydrochloric acid / sodium hydroxide solution, which is a conventional practice in the art and therefore not specifically limited in this embodiment of the invention.

[0102] In some specific embodiments, in step s102 above, the immersion rolling process is two immersions and two rollings.

[0103] In some specific embodiments, in step s102 above, the roll residue of the immersion rolling process is 70%~80%.

[0104] In some embodiments, in step s102 above, the pre-baking temperature is 100°C to 110°C.

[0105] In some embodiments, the pre-baking time in step s102 is 3 min to 5 min.

[0106] In some embodiments, in step s102 above, the baking temperature is 150°C to 160°C.

[0107] In some embodiments, the baking time in step s102 is 2 min to 3 min.

[0108] In some embodiments, in step s10 above, the grafting treatment of component B includes the following steps: s103.B component is diluted with water to obtain diluted B solution.

[0109] s104. The fabric is impregnated with diluted solution B and then dried.

[0110] In some embodiments, in step s103 above, the solid content of diluent B is 3% to 5%.

[0111] In some embodiments, in step s103 above, the pH value of diluent B is 6.5~7.5. It should be noted that the pH value of diluent B can be adjusted using dilute hydrochloric acid / sodium hydroxide solution, which is a conventional practice in the art and therefore not specifically limited in this embodiment of the invention.

[0112] In some embodiments, in step s104 above, the temperature of the impregnation treatment is 50°C to 60°C.

[0113] In some embodiments, the immersion treatment time in step s104 above is 20 min to 30 min.

[0114] In some embodiments, in step s104 above, the bath ratio in the impregnation process is 1:(10~15).

[0115] In some embodiments, in step s104 above, the drying temperature is 80°C to 100°C.

[0116] The following description, in conjunction with specific embodiments, provides further details. For ease of explanation, the following embodiments and comparative examples are as follows: (1) The CAS number of isophorone diisocyanate is 4098-71-9.

[0117] (2) Polycaprolactone diol is PCL-2000.

[0118] (3) The CAS number of hydroxyl-terminated polysiloxane is 156327-07-0.

[0119] (4) The CAS number of N-methyldiethanolamine is 105-59-9.

[0120] (5) The CAS number of bisphenol A (2,3-dihydroxypropyl) glycidyl is 76002-91-0.

[0121] (6) The CAS number of dibutyltin dilaurate is 105124-36-5.

[0122] (7) The CAS number of polyethylene glycol is 25322-68-3.

[0123] (8) The CAS number of fatty alcohol polyoxyethylene ether is 68213-23-0.

[0124] Example 1 Example 1 provides a two-component anti-dyeing agent, consisting of component A and component B.

[0125] Component A consists of components at the following concentrations: 170 g / L isophorone diisocyanate, 120 g / L polycaprolactone diol, 70 g / L hydroxyalkyl-terminated polysiloxane, 40 g / L N-methyldiethanolamine, 30 g / L bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 1.5 g / L dibutyltin dilaurate, with the balance being water.

[0126] Component B consists of components at the following concentrations: 180 g / L water-soluble modified polyester, 100 g / L polyethylene glycol, 60 g / L fatty alcohol polyoxyethylene ether, with the balance being water; The water-soluble modified polyester is sulfonated polyethylene terephthalate. The raw materials for its preparation consist of mixed diacids, ethylene glycol, antimony trioxide, and triphenyl phosphate. The molar ratio of the mixed diacids to ethylene glycol is 1:1.3, and the mass of triphenyl phosphate is 0.01% of the total mass of the mixed diacids and ethylene glycol. The mixed dicarboxylic acid is composed of the following components by mass fraction: 85% terephthalic acid, 15% sodium isophthalate-5-sulfonate; The amount of antimony trioxide used is 0.04% of the mass of terephthalic acid.

[0127] This embodiment also provides a method for preparing the above-mentioned two-component anti-dyeing agent, the steps of which are as follows: Preparation of component E10.A E101. First mixing treatment: Polycaprolactone diol is dehydrated under vacuum, then mixed with isophorone diisocyanate and dibutyltin dilaurate for catalytic reaction, and then mixed with hydroxyalkyl-terminated polysiloxane for further reaction to obtain a prepolymer; The vacuum dehydration process was carried out at a temperature of 120℃, a time of 2 hours, and a pressure of -0.1MPa. The temperature for the mixed catalytic reaction was 80℃ and the time was 2 hours. The reaction continued for 1.5 hours.

[0128] E102. Second mixing treatment: After the prepolymer and N-methyldiethanolamine are mixed and reacted, bisphenol A (2,3-dihydroxypropyl) glycidyl ether is added and reacted to obtain the polymer; The reaction temperature of the prepolymer and N-methyldiethanolamine was 60℃ and the time was 1 hour. The reaction time for adding bisphenol A (2,3-dihydroxypropyl) glycidyl ether was 2 hours. E103. Post-treatment: After mixing the polymer and glacial acetic acid (0.8 times the volume of the polymer) for 15 min, emulsify with deionized water under high-speed shear at 3000 rpm, and then perform vacuum distillation to obtain component A; finally, adjust the pH of component A to 5 with hydrochloric acid.

[0129] Preparation of component E20.B E201. Preparation of water-soluble modified polyester: Under a nitrogen atmosphere, a mixture of diacid, ethylene glycol and antimony trioxide is esterified and then mixed with triphenyl phosphate for polycondensation treatment to obtain a water-soluble modified polyester. The esterification treatment was carried out at a temperature of 220℃, a pressure of 0.2MPa, and a time of 2h. The polycondensation treatment was carried out at a temperature of 270℃, a pressure of 90Pa, and a time of 2h.

[0130] E202. Preparation of the mixed system: After heating water to 65°C, polyethylene glycol and the prepared water-soluble modified polyester are added to obtain the mixed system.

[0131] E203. Mixing: After the mixture is cooled to 40°C, it is mixed with fatty alcohol polyoxyethylene ether and stirred for 30 minutes.

[0132] E204. Adjust pH value: Adjust the pH value of component B to 6 using sodium hydroxide solution.

[0133] Example 2 Example 2 provides a two-component anti-dyeing agent, consisting of component A and component B.

[0134] Component A consists of components at the following concentrations: 150 g / L isophorone diisocyanate, 100 g / L polycaprolactone diol, 50 g / L hydroxyalkyl-terminated polysiloxane, 30 g / L N-methyldiethanolamine, 20 g / L bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 1 g / L dibutyltin dilaurate, with the balance being water.

[0135] Component B consists of components at the following concentrations: 150 g / L water-soluble modified polyester, 80 g / L polyethylene glycol, 50 g / L fatty alcohol polyoxyethylene ether, with the balance being water; The water-soluble modified polyester is sulfonated polyethylene terephthalate. The raw materials for its preparation consist of mixed diacids, ethylene glycol, antimony trioxide, and triphenyl phosphate. The molar ratio of the mixed diacids to ethylene glycol is 1:1.2, and the mass of triphenyl phosphate is 0.01% of the total mass of the mixed diacids and ethylene glycol. The mixed dicarboxylic acid is composed of the following components by mass fraction: 85% terephthalic acid, 15% sodium isophthalate-5-sulfonate; The amount of antimony trioxide used is 0.03% of the mass of terephthalic acid.

[0136] This embodiment also provides a method for preparing the above-mentioned two-component anti-dyeing agent, with the same steps as in Example 1.

[0137] Example 3 Example 3 provides a two-component anti-dyeing agent, consisting of component A and component B.

[0138] Component A consists of components at the following concentrations: 200 g / L isophorone diisocyanate, 150 g / L polycaprolactone diol, 80 g / L hydroxyalkyl-terminated polysiloxane, 50 g / L N-methyldiethanolamine, 40 g / L bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 2 g / L dibutyltin dilaurate, with the balance being water.

[0139] Component B consists of components at the following concentrations: 200 g / L water-soluble modified polyester, 120 g / L polyethylene glycol, 80 g / L fatty alcohol polyoxyethylene ether, with the balance being water; The water-soluble modified polyester is sulfonated polyethylene terephthalate. The raw materials for its preparation consist of mixed diacids, ethylene glycol, antimony trioxide, and triphenyl phosphate. The molar ratio of the mixed diacids to ethylene glycol is 1:1.5, and the mass of triphenyl phosphate is 0.02% of the total mass of the mixed diacids and ethylene glycol. The mixed dicarboxylic acid is composed of the following components by mass fraction: 85% terephthalic acid, 15% sodium isophthalate-5-sulfonate; The amount of antimony trioxide used is 0.05% of the mass of terephthalic acid.

[0140] This embodiment also provides a method for preparing the above-mentioned two-component anti-dyeing agent, with the same steps as in Example 1.

[0141] Comparative Example 1 Comparative Example 1 provides an anti-dyeing agent consisting only of component B from Example 1.

[0142] Comparative Example 2 Comparative Example 2 provides an anti-dyeing agent composed of components at the following concentrations: 180 g / L polyethylene terephthalate (CAS No.: 25038-59-9), 100 g / L polyethylene glycol, 60 g / L fatty alcohol polyoxyethylene ether, with the balance being water.

[0143] To verify the advancement of the two-component anti-dyeing agent and its preparation method provided in this embodiment of the invention, the two-component anti-dyeing agent provided in the embodiment and the anti-dyeing agent provided in the comparative example were tested on the color and elasticity protection of denim fabric, and the results are shown in Table 1 below.

[0144] The testing steps for the color and elasticity protection of denim fabric are as follows: e10. Sample selection: Select indigo-dyed denim fabric (K / S value > 12) that has not been washed as a sample.

[0145] e20. Anti-dyeing treatment e201. Component A treatment (this step is not required for Comparative Examples 1 and 2): (1) Component A is diluted with water and the pH value is adjusted with hydrochloric acid to obtain diluted solution A; the solid content of diluted solution A is 8% and the pH value is 5.

[0146] (2) After the fabric is dipped and rubbed twice with diluted solution A (with a 70% rub rate), it is pre-dried at 100°C for 3 minutes and then heated to 150°C for 2 minutes to obtain denim fabric treated with component A.

[0147] e202.B component treatment (1) Component B was diluted with water and the pH value was adjusted with sodium hydroxide solution to obtain diluted solution B; the solid content of diluted solution B was 4% and the pH value was 7.

[0148] (2) The denim fabric was immersed in diluted solution B at 50°C for 20 minutes and then dried at 80°C to obtain denim fabric treated with anti-dyeing agent; the bath ratio in the immersion treatment was 1:13.

[0149] e30. Staining test (1) Experimental group: denim fabric treated with anti-dyeing agent.

[0150] Blank control group: Take another identical sample and do not treat it with any anti-dyeing agent.

[0151] White backing: Standard multifiber backing fabric (such as DW type) or white cotton fabric, used for visual assessment of staining levels.

[0152] (2) Sew the experimental group and the blank control group together with white lining respectively.

[0153] 1) Prepare a water bath: 6 g of neutral cellulase, 2 g of polyester polyether, 40 kg of water, and raise the water temperature to 60℃.

[0154] 2) Place both sets of combined samples into the washing sample machine at the same time and process for 120 minutes.

[0155] 3) After removing it, remove the white backing, rinse it with clean water and let it air dry; 4) Detect the K / S value of white backing: At the maximum absorption wavelength of indigo, 660nm, the colorimetric data of the same sample were calculated and the average value of 5 test results was taken. The lower the K / S value, the better the anti-re-dyeing effect. The results are shown in Table 1 below.

[0156] e103. Removal of anti-dyeing agent The denim fabric treated with anti-dyeing agent was immersed in sodium carbonate solution (concentration 2g / L) with a liquor ratio of 1:15 and the temperature was adjusted to 70℃ for 15 minutes. After the denim fabric was dehydrated and dried, the stretch and resilience of the denim fabric was tested. The results are shown in Table 1 below.

[0157]

[0158] From the table above, at least the following conclusions can be drawn: The anti-dyeing agent in Comparative Example 1 does not contain component A, which protects the denim fabric. Its anti-dyeing effect is not significantly different from the example, but its stretch and resilience are worse. The anti-dyeing agent in Comparative Example 2 does not contain component A and uses unmodified polyethylene terephthalate. Its anti-dyeing effect and stretch and resilience are both severely reduced, especially its anti-dyeing effect, which is an order of magnitude lower than the example. Therefore, the two-component anti-dyeing agent provided in this invention uses component A as the bottom layer material. This protects the fabric from polyester residue in component B, preventing problems such as fabric stiffness. Removal only requires alkaline conditions, where the quaternary ammonium cation (-NR3) of component A... + ) by OH - Neutralization transforms the component into a free amine (-NR3), the positive charge disappears, and the B component, which loses electrostatic attraction, detaches from the fiber surface and enters the aqueous phase to be washed away. It can also firmly graft the B component to form a hydrophilic barrier layer on the fiber surface, preventing dye molecules (especially disperse dyes) from contacting the fiber. At the same time, the hydration of the PEG chain segments enhances the anti-dyeing effect.

[0159] It should be noted that the present invention is not limited to the above-described embodiments. The above embodiments are merely examples, and any embodiments that have the same structure and perform the same effects as the technical concept within the scope of the present invention are included within the scope of the present invention. Furthermore, various modifications that can be conceived by those skilled in the art to the embodiments, and other ways of constructing by combining some of the constituent elements of the embodiments, without departing from the spirit of the present invention, are also included within the scope of the present invention.

Claims

1. A two-component anti-dyeing agent, characterized in that, Includes component A and component B; Component A includes components at the following concentrations: 150g / L~200g / L isophorone diisocyanate, 100g / L~150g / L polycaprolactone diol, 50g / L~80g / L hydroxyalkyl-terminated polysiloxane, 30g / L~50g / L N-methyldiethanolamine, 20g / L~40g / L bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 1g / L~2g / L dibutyltin dilaurate; Component B includes components at the following concentrations: 150g / L~200g / L water-soluble modified polyester, 80g / L~120g / L polyethylene glycol, 50g / L~80g / L fatty alcohol polyoxyethylene ether.

2. The two-component anti-dyeing agent according to claim 1, characterized in that, The water-soluble modified polyester is sulfonated polyethylene terephthalate, and the raw materials for preparing the sulfonated polyethylene terephthalate include mixed diacids and ethylene glycol.

3. The two-component anti-dyeing agent according to claim 2, characterized in that, It satisfies at least one of the following characteristics (1) to (6): (1) The molar ratio of the mixed dicarboxylic acid and ethylene glycol is 1:1.2~1.5; (2) The mixed dicarboxylic acid comprises the following components in the indicated mass fractions: 85%~90% terephthalic acid, 10%~15% sodium isophthalic acid-5-sulfonate; (3) The raw materials for preparing the sulfonated polyethylene terephthalate also include antimony trioxide; (4) The amount of antimony trioxide used is 0.03%~0.05% of the mass of terephthalic acid; (5) The raw materials for preparing the sulfonated polyethylene terephthalate also include triphenyl phosphate; (6) The mass of triphenyl phosphate is 0.01% to 0.02% of the total mass of the mixed dicarboxylic acid and ethylene glycol.

4. A method for preparing a two-component anti-dyeing agent as described in any one of claims 1 to 3, characterized in that, Includes the following steps: Prepare component A and component B separately.

5. The method for preparing the two-component anti-dyeing agent according to claim 4, characterized in that, The preparation of component B includes the following steps: Mix water-soluble modified polyester, polyethylene glycol, fatty alcohol polyoxyethylene ether and water according to the preset concentration.

6. The method for preparing the two-component anti-dyeing agent according to claim 5, characterized in that, The preparation of the water-soluble modified polyester includes the following steps: The mixture of diacid, ethylene glycol and antimony trioxide was esterified and then mixed with triphenyl phosphate for polycondensation. The mixed dicarboxylic acids include terephthalic acid and sodium isophthalic acid-5-sulfonate.

7. The method for preparing the two-component anti-dyeing agent according to claim 6, characterized in that, It satisfies at least one of the following characteristics (1) to (7): (1) The esterification treatment temperature is 220℃~240℃; (2) The pressure of the esterification treatment is 0.2 MPa to 0.3 MPa; (3) The esterification treatment time is 2h~3h; (4) The temperature of the polycondensation treatment is 260℃~280℃; (5) The pressure of the polycondensation treatment is below 100 Pa; (6) The polycondensation treatment time is 1.5h~2.5h; (7) The step of mixing water-soluble modified polyester, polyethylene glycol, fatty alcohol polyoxyethylene ether and water includes the following steps: After heating water to 60℃~70℃, polyethylene glycol and water-soluble modified polyester are added to obtain a mixed system; After the mixture is cooled to 40℃~45℃, it is mixed and stirred with fatty alcohol polyoxyethylene ether.

8. The method for preparing the two-component anti-dyeing agent according to any one of claims 4 to 7, characterized in that, The preparation of component A includes the following steps: Isophorone diisocyanate, polycaprolactone diol, hydroxyalkyl-terminated polysiloxane and dibutyltin dilaurate were subjected to a first mixing treatment to obtain a prepolymer; The prepolymer, N-methyldiethanolamine, and bisphenol A (2,3-dihydroxypropyl) glycidyl ether were subjected to a second mixing treatment to obtain the polymer.

9. The method for preparing the two-component anti-dyeing agent according to claim 8, characterized in that, It satisfies at least one of the following characteristics (1) to (11): (1) The first mixing process includes the following steps: After vacuum dehydration, polycaprolactone diol is mixed with isophorone diisocyanate and dibutyltin dilaurate for catalytic reaction, and then mixed with hydroxyalkyl-terminated polysiloxane for further reaction. (2) The temperature for vacuum dehydration is 115℃~125℃; (3) The pressure for vacuum dehydration is -0.2MPa to -0.1MPa; (4) The vacuum dehydration time is 2h~3h; (5) The temperature for the mixed catalytic reaction is 75℃~85℃; (6) The time for the mixed catalytic reaction is 2h~3h; (7) The mixing and reaction should continue for 1.5h to 2h; (8) The second mixing process includes the following steps: After the prepolymer and N-methyldiethanolamine are mixed and reacted, bisphenol A (2,3-dihydroxypropyl) glycidyl ether is added and reacted. (9) The reaction temperature of the prepolymer and N-methyldiethanolamine is 55℃~65℃; (10) The reaction time of the prepolymer and N-methyldiethanolamine is 1h~2h; (11) The reaction time for adding bisphenol A (2,3-dihydroxypropyl) glycidyl ether is 2h~3h.

10. A method for treating a fabric, characterized in that, This includes treating the fabric with the two-component anti-dyeing agent as described in any one of claims 1 to 3.

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