Cationic repellent finish for cotton fabric

By preparing a cationic waterborne polyurethane-modified polyacrylate hydrophobic agent, the problem of insufficient toughness and water resistance of existing cotton fabric hydrophobic agents was solved, thereby improving the flexibility and hydrophobic effect of the fabric and enhancing the adhesion and durability of the treatment agent.

CN119553503BActive Publication Date: 2025-11-07BENGBU ADITYA NEW MATERIAL CO LTD +1
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Patent Information

Application Number
CN202411702371.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-26
Publication Date
2025-11-07
Estimated Expiration
2044-11-26

AI Technical Summary

Technical Problem

Existing water-repellent treatment agents for cotton fabrics are insufficient in terms of toughness and water resistance, which affects their application range and performance stability.

Method used

A hydrophobic treatment agent with good flexibility and hydrophobic effect was prepared by using cationic waterborne polyurethane modified polyacrylate as a hydrophobic treatment agent and reacting fluorinated silicone modified isocyanate with polytetrahydrofuran diol, combined with dynamic oxime-carbamate bonds and double bond chain extenders.

Benefits of technology

It improves the hydrophobicity of cotton fabrics and the binding force of the treatment agent, enhances the fabric's flexibility and durability, while maintaining the fabric's hand feel and breathability.

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Abstract

The application relates to the technical field of fine polymer materials, and discloses a cationic hydrophobic treatment agent for cotton fabric, which comprises the following raw materials: modified isocyanate, polytetrahydrofuran glycol, double-bond type chain extender, tertiary amine type chain extender, dynamic bond type chain extender, octadecyl methacrylate, organic tin catalyst and azobisdimethylamidin hydrochloride. Based on the hydrophilic and hydrophobic parts connected by the dynamic oxime-urethane bond between chains, the hydrophilic and hydrophobic components exhibit phase separation, thereby improving the hydrophobic performance of the coating. In addition, the double bond structure between the polymer chains can be used to introduce long-chain alkyl groups to form a brush structure and improve the hydrophobic performance of the coating. Meanwhile, the fabric is negatively charged after dyeing treatment, can be combined with the cationic latex in the cationic water-based polyurethane, and the adhesion of the hydrophobic treatment agent on the fabric is improved. The hydrophobic treatment agent prepared by the application has the characteristics of good flexibility and good hydrophobic effect after treating the cotton fabric, and can promote the related industry to achieve breakthrough development.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of fine polymer materials, in particular to a cationic hydrophobic treatment agent for cotton fabric. BACKGROUND

[0002] Cotton fabric is a natural fiber fabric with the largest use at present, has good dyeing performance and comfortable wearing characteristics, is one of the best choices for clothing, home textiles and industrial textiles, but the hydrophilicity of untreated cotton fabric is relatively strong, which leads to easy contamination, breeding of bacteria and other microorganisms, and these disadvantages limit the use range of cotton fabric, therefore, the cotton fabric with hydrophobic property will be an important content to expand the application field of cotton fabric.

[0003] Using hydrophobic treatment agent is an important method to improve the hydrophobic effect of cotton fabric, and the organic fluorine has good thermal stability and chemical properties, can reduce the surface energy of the fabric, so that the oil, water and stains cannot be infiltrated to a certain extent, and does not affect the hand feeling, air permeability and other properties of the fabric.

[0004] Patent document CN102675527A reports a water-based hydrophobic agent prepared by emulsifying reaction of long-chain acrylate monomer, which has the advantages of not easy to migrate, good stability, good isolation effect, but its toughness and water resistance are poor, which limits its application. In addition, patent document CN101962514A reports a long-durable super-hydrophobic self-cleaning coating material prepared by polysiloxane, which realizes the super-hydrophobic self-cleaning coating with lotus effect by using the photocatalytic decomposition characteristics of nanoparticles on organic pollutants, is suitable for large-area construction and has good weather resistance, but the nanoparticles are easy to agglomerate, which affects the function of the coating. SUMMARY

[0005] (I) Technical problems to be solved

[0006] In view of the deficiencies of the prior art, the present application provides a cationic hydrophobic treatment agent for cotton fabric, which has good flexibility and good hydrophobic effect after treating the cotton fabric.

[0007] (II) Technical solutions

[0008] A cationic hydrophobic treatment agent for cotton fabric, the hydrophobic treatment agent is a cationic water-based polyurethane modified polyacrylate, which comprises the following components in mole:

[0009] fluorine-containing silicon modified isocyanate 100 parts, polytetrahydrofuran glycol (PTMG) 40-60 parts, dynamic bond type chain extender 10-20 parts, tertiary amine type chain extender 30 parts, double bond type chain extender 10-30 parts, octadecyl methacrylate (SMA) 100-300 parts, organic tin catalyst 0.2 parts, azobisdimethylamidinum hydrochloride (AIBA) 0.2-0.5 parts;

[0010] The polytetrahydrofuran glycol has a molecular weight M = 1000 g / mol.

[0011] The dynamic bond type chain extender is dimethylglyoxime (DMG).

[0012] The tertiary amine type chain extender is N-methyldiethanolamine (MDEA).

[0013] The double bond type chain extender is 2,3-dihydroxypropyl acrylate (GMMA).

[0014] The organic tin catalyst is dibutyltin dilaurate (DBTDL).

[0015] The preparation method of the cationic hydrophobic treatment agent for cotton fabric is as follows:

[0016] (1) Under a nitrogen atmosphere, fluorine-containing silicon modified isocyanate and polytetrahydrofuran glycol are added to a flask, and stirred at 80°C for 2 hours to obtain an isocyanate-terminated prepolymer.

[0017] (2) After the prepolymer is cooled to 45°C, chain extension of the prepolymer is achieved by adding MDEA and DBTAL dissolved in acetone to obtain a cationic prepolymer.

[0018] (3) GMMA dissolved in acetone is continuously added to the cationic prepolymer, heated to 65°C and reacted for 2 hours, then DMG dissolved in acetone is added to complete the chain extension reaction.

[0019] (4) The chain-extended prepolymer is cooled to room temperature and neutralized with acetic acid.

[0020] (5) SMA is added, and deionized water is slowly added under vigorous stirring for emulsification.

[0021] (6) The temperature is raised to 75°C, and the initiator AIBA dissolved in water is added dropwise to the emulsion, and reacted for 6 hours. After the reaction is completed, a cationic hydrophobic treatment agent is obtained.

[0022] Preferably, in step (2), 1 mass part of MDEA is dissolved in 1-3 mass parts of acetone solvent.

[0023] Preferably, in the step (3), the GMMA dissolved in acetone is 1 mass fraction of GMMA dissolved in 1-3 mass fractions of acetone solvent; the DMG dissolved in acetone is 1 mass fraction of DMG dissolved in 1-3 mass fractions of acetone solvent.

[0024] Preferably, the preparation method of the fluorine-containing silicon-modified isocyanate is:

[0025] A1, under a nitrogen atmosphere, 1,6-divinyl perfluorohexane, 1% mass fraction of chloroplatinic acid isopropanol solution is added to a flask, stirred and dispersed, heated to 120-130℃, and heptamethyltrisiloxane is added, stirred and reacted for 6-12h, after the reaction is completed, rotary evaporation is carried out to obtain intermediate 1;

[0026] A2, intermediate 1 and diethanolamine are added to isopropanol solvent, stirred and dispersed, heated to 75-82℃, reacted for 1-3h, after the reaction is completed, deionized water is washed, and dried to obtain intermediate 2;

[0027] A3, intermediate 2 and isophorone diisocyanate are added to N,N-dimethylformamide solvent, stirred and mixed uniformly, heated to 70-80℃, and dibutyltin dilaurate is added, reacted for 3-6h, after the reaction is completed, deionized water is washed, and dried to obtain the fluorine-containing silicon-modified isocyanate.

[0028] Further preferably, in the A1, the molar ratio of 1,6-divinyl perfluorohexane to heptamethyltrisiloxane is 1:0.8-1.

[0029] Further preferably, in the A2, the molar ratio of intermediate 1 to diethanolamine is 1:1-1.5.

[0030] Further preferably, in the A3, the molar ratio of intermediate 2 to isophorone diisocyanate to dibutyltin dilaurate is 1:2-2.4:0.005-0.01.

[0031] (Three) beneficial technical effects

[0032] (1) The hybrid emulsion of water-based cationic polyurethane and long carbon chain polyacrylate is used for hydrophobic treatment agent material, which has the characteristics of good compatibility, stable performance, good flexibility and hydrophobic effect, and the fabric after treatment has comfortable hand feeling.

[0033] (2) The surface of cotton fabric generally has a negative charge, which can be combined with the cationic latex in the cationic waterborne polyurethane, thereby improving the binding force of the hydrophobic treatment agent on the fabric. By reacting the oxime group with the isocyanate group, a reversible dynamic oxime-urethane bond is introduced into the main chain of the cationic waterborne polyurethane, which is dissociated at high-temperature finishing, and the free isocyanate group can be irreversibly reacted with the hydroxyl group on the surface of the fabric, thereby improving the adhesion and durability of the treatment agent on the fabric.

[0034] (3) By introducing a double bond type chain extender, a carbon-carbon double bond is introduced into the polyurethane main chain, and an octadecyl structure is grafted at the double bond. Under high-temperature conditions, the dynamic oxime-urethane bond of the polyurethane main chain will dissociate and recombine, and the long alkyl chain part with low surface energy and the fluorosilicon group are more likely to migrate to the surface, thereby producing excellent hydrophobic properties. BRIEF DESCRIPTION OF DRAWINGS

[0035] Figure 1 is the reaction route of the fluorosilicon-containing modified isocyanate. DETAILED DESCRIPTION

[0036] The specific embodiments of the present application are described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present application, and are not used to limit the scope of the present application.

[0037] In the examples, isophorone diisocyanate was purchased from BASF SE; polytetrahydrofuran diol was purchased from Hefei Tianjian Chemical Co., Ltd.; dibutyltin dilaurate and octadecyl methacrylate, azobisdimethylvaleronitrile, 2,3-dihydroxypropyl acrylate, 1,6-divinyl perfluorohexane, diethanolamine, were all purchased from Aldrich Reagent Co., Ltd.; butanedione oxime was purchased from Macklin Biochemical Technology Co., Ltd.; N-methyldiethanolamine was purchased from Alpha Aesar (China) Chemical Co., Ltd.

[0038] Example 1

[0039] (1) Under a nitrogen atmosphere, 1 mol of 1,6-divinyl perfluorohexane and 10 mL of 1% by mass isopropyl alcohol solution of chloroplatinic acid were added to a flask, stirred and dispersed, heated to 125°C, and 0.8 mol of heptamethyltrisiloxane was added thereto, stirred and reacted for 10 h. After the reaction was completed, rotary evaporation was performed to obtain intermediate 1.

[0040] (2) 0.5 mol of intermediate 1 and 0.75 mol of diethanolamine were added to 50 mL of isopropyl alcohol solvent, stirred and dispersed, heated to 75°C, and reacted for 1 h. After the reaction was completed, deionized water was used for washing and drying to obtain intermediate 2.

[0041] (3) 0.01 mol of intermediate 2, 0.022 mol of isophorone diisocyanate were added to 50 mL of N,N-dimethylformamide solvent, stirred and mixed uniformly, warmed to 75°C, 0.08 mmol of dibutyltin dilaurate was added thereto, reacted for 3 h, after the reaction was completed, washed with deionized water, dried, and a fluorine-containing silicon-modified isocyanate was obtained.

[0042] (4) 0.1 mol of the fluorine-containing silicon-modified isocyanate and 0.06 mol of polytetrahydrofuran diol were added to a flask under a nitrogen atmosphere, stirred and reacted for 2 h at 80°C, and an isocyanate-terminated prepolymer was obtained.

[0043] (5) After the above prepolymer was cooled to 45°C, chain extension of the prepolymer was performed by adding 0.01 mol of MDEA and 0.2 mmol of DBTAL dissolved in 3 mL of acetone, and a cationic prepolymer was obtained.

[0044] (6) To the cationic prepolymer, 0.02 mol of GMMA dissolved in 5 mL of acetone was further added, warmed to 65°C and reacted for 2 h, and then 0.01 mol of DMG dissolved in 3 mL of acetone was added and the chain extension reaction was completed by further reacting for 2 h.

[0045] (7) The chain-extended prepolymer was lowered to room temperature, and 0.009 mol of acetic acid was added for neutralization.

[0046] (8) 0.2 mol of SMA was added, and 611 mL of deionized water was slowly added under vigorous stirring for emulsification.

[0047] (9) The temperature was warmed to 75°C, and 0.2 mmol of initiator AIBA dissolved in water was added dropwise to the emulsion, and reacted for 6 h, and after the reaction was completed, a cationic water-repellent treatment agent was obtained.

[0048] Example 2

[0049] (1) 1 mol of 1,6-divinylperfluorohexane, 10 mL of a 1% by mass isopropyl alcohol solution of chloroplatinic acid were added to a flask under a nitrogen atmosphere, stirred and dispersed, warmed to 130°C, and 1 mol of heptamethyltrisiloxane was added thereto, stirred and reacted for 6 h, and after the reaction was completed, rotary evaporation was performed, and intermediate 1 was obtained.

[0050] (2) 0.5 mol of intermediate 1, 0.6 mol of diethanolamine were added to 50 mL of isopropyl alcohol solvent, stirred and dispersed, warmed to 80°C, and reacted for 2 h, and after the reaction was completed, washed with deionized water, dried, and intermediate 2 was obtained.

[0051] (3) 0.01 mol of intermediate 2, 0.02 mol of isophorone diisocyanate were added to 50 mL of N,N-dimethylformamide solvent, stirred and mixed uniformly, warmed to 70°C, 0.1 mmol of dibutyltin dilaurate was added thereto, reacted for 6 h, after the reaction was completed, washed with deionized water, dried, and a fluorine-containing silicon-modified isocyanate was obtained.

[0052] (4) 0.1 mol of the fluorine-containing silicon-modified isocyanate and 0.05 mol of polytetrahydrofuran diol were added to a flask under a nitrogen atmosphere, stirred and reacted at 80°C for 2 h, and an isocyanate-terminated prepolymer was obtained.

[0053] (5) After the above prepolymer was cooled to 45°C, chain extension of the prepolymer was performed by adding 0.01 mol of MDEA and 0.2 mmol of DBTAL dissolved in 3 mL of acetone, and a cationic prepolymer was obtained.

[0054] (6) To the cationic prepolymer, 0.02 mol of GMMA dissolved in 5 mL of acetone was further added, warmed to 65°C and reacted for 2 h, and then 0.02 mol of DMG dissolved in 3 mL of acetone was added and the chain extension reaction was completed by further reacting for 2 h.

[0055] (7) The chain-extended prepolymer was lowered to room temperature, and 0.009 mol of acetic acid was added for neutralization.

[0056] (8) 0.2 mol of SMA was added, and 576 mL of deionized water was slowly added under vigorous stirring for emulsification.

[0057] (9) The temperature was warmed to 75°C, and 0.2 mol of initiator AIBA dissolved in water was added dropwise to the emulsion, and reacted for 6 h to obtain a cationic water-repellent treatment agent.

[0058] Example 3

[0059] (1) 1 mol of 1,6-divinylperfluorohexane, 10 mL of a 1% by mass isopropyl alcohol solution of chloroplatinic acid were added to a flask under a nitrogen atmosphere, stirred and dispersed, warmed to 120°C, and 0.9 mol of heptamethyltrisiloxane was added thereto, stirred and reacted for 12 h, after the reaction was completed, rotary evaporation was performed, and intermediate 1 was obtained.

[0060] (2) 0.5 mol of intermediate 1, 0.5 mol of diethanolamine were added to 50 mL of isopropyl alcohol solvent, stirred and dispersed, warmed to 82°C, and reacted for 3 h, after the reaction was completed, washed with deionized water, dried, and intermediate 2 was obtained.

[0061] (3) 0.01 mol of intermediate 2, 0.24 mol of isophorone diisocyanate were added to 50 mL of N,N-dimethylformamide solvent, stirred and mixed uniformly, warmed to 80°C, 0.05 mmol of dibutyltin dilaurate was added thereto, reacted for 5 h, after the reaction was completed, washed with deionized water, dried, and a fluorine-containing silicon-modified isocyanate was obtained.

[0062] (4) 0.1 mol of the fluorine-containing silicon-modified isocyanate and 0.05 mol of polytetrahydrofuran diol were added to a flask under a nitrogen atmosphere, stirred and reacted at 80°C for 2 h, and an isocyanate-terminated prepolymer was obtained.

[0063] (5) After the above prepolymer was cooled to 45°C, chain extension of the prepolymer was performed by adding 0.01 mol of MDEA and 0.2 mol of DBTAL dissolved in 3 mL of acetone, and a cationic prepolymer was obtained.

[0064] (6) To the cationic prepolymer, 0.01 mol of GMMA dissolved in 3 mL of acetone was further added, warmed to 65°C and reacted for 2 h, and then 0.02 mol of DMG dissolved in 3 mL of acetone was added and the reaction was continued for 2 h to complete the chain extension reaction.

[0065] (7) The chain-extended prepolymer was lowered to room temperature, and 0.009 mol of acetic acid was added for neutralization.

[0066] (8) 0.1 mol of SMA was added, and 437 mL of deionized water was slowly added under vigorous stirring for emulsification.

[0067] (9) The temperature was warmed to 75°C, and 0.2 mmol of initiator AIBA dissolved in water was added dropwise to the emulsion, and the reaction was continued for 6 h to obtain a cationic water-repellent treatment agent.

[0068] Example 4

[0069] (1) 1 mol of 1,6-divinylperfluorohexane, 10 mL of a 1% by mass isopropyl alcohol solution of chloroplatinic acid were added to a flask under a nitrogen atmosphere, stirred and dispersed, warmed to 130°C, and 0.9 mol of heptamethyltrisiloxane was added thereto, stirred and reacted for 10 h, after the reaction was completed, rotary evaporation was performed, and intermediate 1 was obtained.

[0070] (2) 0.5 mol of intermediate 1, 0.6 mol of diethanolamine were added to 50 mL of isopropyl alcohol solvent, stirred and dispersed, warmed to 78°C, and reacted for 2 h, after the reaction was completed, washed with deionized water, dried, and intermediate 2 was obtained.

[0071] (3) 0.01 mol of intermediate 2, 0.022 mol of isophorone diisocyanate were added to 50 mL of N,N-dimethylformamide solvent, stirred and mixed uniformly, warmed to 75°C, 0.06 mmol of dibutyltin dilaurate was added thereto, reacted for 4 h, after the reaction was completed, washed with deionized water, dried, and a fluorine-containing silicon-modified isocyanate was obtained.

[0072] (4) 0.1 mol of the fluorine-containing silicon-modified isocyanate and 0.04 mol of polytetrahydrofuran diol were added to a flask under a nitrogen atmosphere, stirred and reacted at 80°C for 2 h, and an isocyanate-terminated prepolymer was obtained.

[0073] (5) After the above prepolymer was cooled to 45°C, chain extension of the prepolymer was performed by adding 0.01 mol of MDEA and 0.2 mol of DBTAL dissolved in 3 mL of acetone, and a cationic prepolymer was obtained.

[0074] (6) To the cationic prepolymer, 0.03 mol of GMMA dissolved in 8 mL of acetone was further added, warmed to 65°C and reacted for 2 h, and then 0.02 mol of DMG dissolved in 5 mL of acetone was added and reacted for 2 h to complete the chain extension reaction.

[0075] (7) The chain-extended prepolymer was lowered to room temperature, and 0.009 mol of acetic acid was added for neutralization.

[0076] (8) 0.3 mol of SMA was added, and 675 mL of deionized water was slowly added under vigorous stirring for emulsification.

[0077] (9) The temperature was warmed to 75°C, and 0.4 mmol of initiator AIBA dissolved in water was added dropwise to the emulsion, and reacted for 6 h, and after the reaction was completed, a cationic water-repellent treatment agent was obtained.

[0078] Comparative Example 1

[0079] This comparative example differs from Example 1 in that 1,4-butanediol (BDO) was used instead of DMG.

[0080] Comparative Example 2

[0081] This comparative example differs from Example 1 in that BDO was used instead of MDEA.

[0082] Comparative Example 3

[0083] This comparative example differs from Example 1 in that BDO was used instead of GMMA.

[0084] Comparative Example 4

[0085] The difference between the present comparative example and Example 1 is that isophorone diisocyanate is used instead of the fluorine-containing silicon-modified isocyanate.

[0086] The cotton fabric is continuously immersed in a pre-dip tank containing the hydrophobic treatment agent for pre-dip treatment, the pre-dip process time is 30 minutes, the pre-dip speed is 10 m / min, then enters the dip machine for dip treatment, the rolling pressure is 50 N, the dip pressure speed is 10 cm / min, finally the dip-treated fabric is baked and shaped at 160℃ for 2 minutes and cooled.

[0087] Hydrophobic property test:

[0088] Test method: the hydrophobic property of the sample is measured by a contact angle measuring instrument at 25℃, the medium is deionized water, the water contact angle of each group of samples at 5 different positions is tested, the highest value and the lowest value are removed, and the average value of the remaining numbers is taken.

[0089] Table 1:

[0090] Pre-wash contact angle (°) Contact angle after 15 washes (°) Example 1 160 139 Example 2 169 148 Example 3 158 132 Example 4 164 143 Comparative Example 1 136 82 Comparative Example 2 141 132 Comparative Example 3 103 88 Comparative Example 4 98 82

[0091] The greater the contact angle, the better the hydrophobicity, and as shown in the table, the hydrophobic agent prepared by the present application has good hydrophobic effect.

[0092] Flexibility test:

[0093] Test method: a 200g weight is pressed on the present example at 25℃, after 1h, the weight is removed and the crease is observed, in order to eliminate errors, a 200g weight is again pressed in the vertical direction of the first crease, after 1h, the weight is removed and the crease is observed.

[0094] Table 2

[0095] Crease performance Example 1 Not noticeable Example 2 Not noticeable Example 3 Not noticeable Example 4 Not noticeable Comparative Example 1 Noticeable Comparative Example 2 Not noticeable Comparative Example 3 Not noticeable Comparative Example 4 More noticeable

[0096] As shown in the table, the hydrophobic treatment agent prepared by the present application can improve the flexibility of the cotton fabric after finishing.

[0097] Emulsion stability test:

[0098] Test method: according to the oven method in GB / T 16497-2007, 100ml of the sample is placed in an 85±1℃ constant temperature oven for 48h, then is placed at room temperature for 1h, the water content in the upper and lower samples is tested according to the method specified in GB / T 11275-2007, so as to determine the stability of the emulsion.

[0099] Emulsion stability Example 1 Stable Example 2 Stable Example 3 Stable Example 4 Stable Comparative Example 1 Stable Comparative Example 2 Stable Comparative Example 3 Unstable Comparative Example 4 Unstable

[0100] As shown in the table, the hydrophobic treatment agent prepared by the present application has good stability.

Claims

1. A cationic hydrophobic treatment for cotton fabrics, characterized in that, The hydrophobic treatment agent is a cationic waterborne polyurethane modified polyacrylate, comprising the following components in moles: fluorine-silicon modified isocyanate 100 parts, polytetramethylene glycol (PTMG) 40-60 parts, dynamic bond type chain extender 10-20 parts, tertiary amine type chain extender 30 parts, double bond type chain extender 10-30 parts, octadecyl methacrylate (SMA) 100-300 parts, organic tin catalyst 0.2 parts, azobisdimethylamino propane hydrochloride (AIBA) 0.2-0.5 parts; The polytetramethylene glycol has a molecular weight M=1000 g / mol; The dynamic bond type chain extender is dimethylglyoxime (DMG); The tertiary amine type chain extender is N-methyldiethanolamine (MDEA); The double bond type chain extender is 2,3-dihydroxypropyl acrylate (GMMA); The organic tin catalyst is dibutyltin dilaurate (DBTDL); The preparation method of the cationic hydrophobic treatment agent for cotton fabric is as follows: (1) under a nitrogen atmosphere, the fluorine-silicon modified isocyanate and the polytetramethylene glycol are added to a flask, stirred and reacted at 80°C for 2 h to obtain an isocyanate-terminated prepolymer; (2) after cooling the prepolymer to 45°C, the prepolymer is chain-extended by adding MDEA and DBTAL dissolved in acetone to obtain a cationic prepolymer; (3) GMMA dissolved in acetone is further added to the cationic prepolymer, heated to 65°C and reacted for 2 h, then DMG dissolved in acetone is added to continue the chain extension reaction for 2 h; (4) the chain-extended prepolymer is cooled to room temperature and neutralized with acetic acid; (5) SMA is added, and deionized water is slowly added under vigorous stirring for emulsification; (6) the temperature is raised to 75°C, and the initiator AIBA dissolved in water is added dropwise to the emulsion, and reacted for 6 h, to obtain the cationic hydrophobic treatment agent; The preparation method of the fluorine-silicon modified isocyanate is as follows: A1, under a nitrogen atmosphere, 1,6-divinyl perfluorohexane and 1% chloroplatinic acid isopropyl alcohol solution are added to a flask, stirred and dispersed, heated to 120-130°C, and heptamethyltrisiloxane is added thereto, stirred and reacted for 6-12 h, after the reaction is completed, rotary evaporation is performed to obtain intermediate 1; A2, intermediate 1 and diethanolamine are added to isopropyl alcohol solvent, stirred and dispersed, heated to 75-82°C, and reacted for 1-3 h, after the reaction is completed, deionized water is washed, and dried to obtain intermediate 2; A3, intermediate 2 and isophorone diisocyanate are added to N,N-dimethylformamide solvent, stirred and mixed uniformly, heated to 70-80°C, and dibutyltin dilaurate is added thereto, reacted for 3-6 h, after the reaction is completed, deionized water is washed, and dried to obtain the fluorine-silicon modified isocyanate.

2. The cationic hydrophobic treatment agent for cotton fabrics according to claim 1, characterized by, In step (2), the MDEA dissolved in acetone is 1 part by mass of MDEA dissolved in 1-3 parts by mass of acetone solvent.

3. The cationic hydrophobic treatment agent for cotton fabrics according to claim 1, characterized by, In the step (3), the GMMA dissolved in acetone is 1 part by mass of GMMA dissolved in 1-3 parts by mass of acetone solvent; the DMG dissolved in acetone is 1 part by mass of DMG dissolved in 1-3 parts by mass of acetone solvent.

4. The cationic hydrophobic treatment agent for cotton fabrics according to claim 1, characterized by, In the A1, the molar ratio of 1,6-divinyl perfluorohexane and heptamethyltrisiloxane is 1:0.8-1.

5. The cationic hydrophobic treatment agent for cotton fabrics according to claim 1, characterized by, In the A2, the molar ratio of intermediate 1 and diethanolamine is 1:1-1.

5.

6. The cationic hydrophobic treatment for cotton fabrics according to claim 1, characterized in that, In the A3, the molar ratio of intermediate 2, isophorone diisocyanate and dibutyltin dilaurate is 1:2-2.4:0.005-0.01.

Citation Information

Patent Citations

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