Cationic hydrophobic treatment agent for cotton fabrics
By using a hybrid emulsion of cationic aqueous polyurethane and long carbon chain polyacrylate as a hydrophobic treatment agent, the shortcomings of the hydrophobic treatment agent in the prior art in terms of toughness and water resistance are solved, and efficient hydrophobic treatment of cotton fabrics is achieved, and its flexibility and stability are improved.
Patent Information
- Application Number
- CN202411702371.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-26
- Publication Date
- 2025-03-04
- Estimated Expiration
- 2044-11-26
AI Technical Summary
In the prior art, hydrophobic treatment agents used in cotton fabrics have shortcomings in toughness and water resistance, which limits their application scope.
A hybrid emulsion of cationic aqueous polyurethane and long carbon chain polyacrylate is used as a hydrophobic treatment agent, and a treatment agent with excellent hydrophobic properties is prepared through specific reaction steps and component ratios.
The hydrophobic treatment agent shows good flexibility and hydrophobic effects on cotton fabrics, and has a comfortable feel and good stability, which is suitable for expanding the application fields of cotton fabrics.
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Figure CN119553503A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of fine polymer materials, in particular to a cationic hydrophobic treating agent for cotton fabrics. Background Art
[0002] Cotton fabric is currently the most widely used natural fiber fabric. It has good dyeing properties and is comfortable to wear. It is one of the best choices for clothing, home textiles and industrial textiles. However, untreated cotton fabric has a strong hydrophilicity, which makes it easy to be stained and breed bacteria and other microorganisms. These disadvantages limit the scope of use of cotton fabrics. Therefore, cotton fabrics with hydrophobic properties will be an important part of expanding the application of cotton fabrics.
[0003] Using hydrophobic treatment agents is an important method to improve the hydrophobic effect of cotton fabrics. Organic fluorine has good thermal stability and chemical properties, which can reduce the surface energy of the fabric to the extent that oil, water, and stains cannot penetrate it, and does not affect the fabric's feel, breathability and other properties.
[0004] Patent document CN102675527A reports a water-based hydrophobic agent prepared by emulsification reaction of long-chain acrylate monomers. This hydrophobic agent has the advantages of not easy to migrate, good stability, and good isolation effect, but its poor toughness and water resistance limit its application. In addition, patent document CN101962514A reports a long-durable super-hydrophobic self-cleaning coating material prepared by polysiloxane. The coating uses the photocatalytic decomposition characteristics of nanoparticles on organic pollutants to achieve a super-hydrophobic self-cleaning coating with a lotus leaf effect. It is suitable for large-area construction and has good weather resistance, but the nanoparticles are prone to agglomeration, which affects the performance of the coating function. Summary of the invention
[0005] 1. Technical issues to be resolved
[0006] In view of the deficiencies of the prior art, the present invention provides a cationic hydrophobic treatment agent for cotton fabrics. After the hydrophobic treatment agent prepared by the present invention is used to treat cotton fabrics, the cotton fabrics have the characteristics of good flexibility, good hydrophobic effect, etc.
[0007] (II) Technical solution
[0008] A cationic hydrophobic treatment agent for cotton fabrics, the hydrophobic treatment agent is a cationic waterborne polyurethane modified polyacrylate, comprising the following components in molar parts:
[0009] 100 parts of fluorine-containing silicon-modified isocyanate, 40-60 parts of polytetramethylene glycol (PTMG), 10-20 parts of dynamic bond type chain extender, 30 parts of tertiary amine type chain extender, 10-30 parts of double bond type chain extender, 100-300 parts of octadecyl methacrylate (SMA), 0.2 parts of organotin catalyst, 0.2-0.5 parts of azobisisobutyramidine hydrochloride (AIBA);
[0010] The molecular weight of the polytetrahydrofuran diol is M=1000 g / mol;
[0011] The dynamic bond type chain extender is dimethylglyoxime (DMG);
[0012] The tertiary amine chain extender is N-methyldiethanolamine (MDEA);
[0013] The double bond type chain extender is 2,3-dihydroxypropyl acrylate (GMMA);
[0014] The organotin 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 diol are added to a flask, and stirred at 80° C. for 2 h to obtain an isocyanate-terminated prepolymer;
[0017] (2) After cooling the prepolymer to 45° C., MDEA and DBTAL dissolved in acetone are added to achieve chain extension of the prepolymer to obtain a cationic prepolymer;
[0018] (3) GMMA dissolved in acetone is continuously added to the cationic prepolymer, the temperature is raised to 65° C. and the reaction is continued for 2 hours, and then DMG dissolved in acetone is added and the reaction is continued for 2 hours to complete the chain extension reaction;
[0019] (4) cooling the chain-extended prepolymer to room temperature and adding acetic acid for neutralization;
[0020] (5) Add SMA and slowly add deionized water under vigorous stirring to emulsify;
[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), the MDEA dissolved in acetone is 1 part by mass of MDEA dissolved in 1-3 parts by mass of acetone solvent.
[0023] Preferably, in the step (3), GMMA dissolved in acetone is prepared by dissolving 1 mass part of GMMA in 1-3 mass parts of acetone solvent; and DMG dissolved in acetone is prepared by dissolving 1 mass part of DMG in 1-3 mass parts of acetone solvent.
[0024] Preferably, the preparation method of the fluorine-containing silicon-modified isocyanate is:
[0025] A1. Under a nitrogen atmosphere, add 1,6-divinylperfluorohexane and 1% by mass chloroplatinic acid isopropanol solution into a flask, stir and disperse, heat to 120-130° C., add heptamethyltrisiloxane, stir and react for 6-12 hours, and after the reaction is completed, rotary evaporate to obtain intermediate 1;
[0026] A2, adding intermediate 1 and diethanolamine to isopropanol solvent, stirring and dispersing, heating to 75-82°C, reacting for 1-3h, washing with deionized water after the reaction, and drying to obtain intermediate 2;
[0027] A3. Add intermediate 2 and isophorone diisocyanate to N,N-dimethylformamide solvent, stir and mix evenly, heat to 70-80°C, add dibutyltin dilaurate thereto, react for 3-6 hours, and after the reaction is completed, wash with deionized water and dry to obtain fluorine-containing silicon-modified isocyanate.
[0028] More preferably, in A1, the molar ratio of 1,6-divinylperfluorohexane to heptamethyltrisiloxane is 1:0.8-1.
[0029] More preferably, in A2, the molar ratio of the intermediate 1 to diethanolamine is 1:1-1.5.
[0030] More preferably, in A3, the molar ratio of intermediate 2, isophorone diisocyanate and dibutyltin dilaurate is 1:2-2.4:0.005-0.01.
[0031] (III) Beneficial technical effects
[0032] (1) The hybrid emulsion of water-based cationic polyurethane and long-chain polyacrylate is used as a hydrophobic treatment agent material. It has the characteristics of good compatibility, stable performance, flexibility and good hydrophobic effect. The treated fabric feels comfortable.
[0033] (2) The surface of cotton fabric generally carries a negative charge, which can combine with the cationic latex in the cationic waterborne polyurethane to improve the binding force of the hydrophobic treatment agent on the fabric. Through the reaction of oxime groups with isocyanate groups, a reversible dynamic oxime-urethane bond is introduced into the main chain of the cationic waterborne polyurethane, which dissociates during high-temperature finishing. The resulting free isocyanate group can react irreversibly 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 onto the double bond. Under high temperature conditions, the dynamic oxime-urethane bond of the polyurethane main chain will dissociate and rebond, and the long alkyl chain part with low surface energy and the fluorosilicone group will migrate to the surface more easily, resulting in excellent hydrophobic properties. BRIEF DESCRIPTION OF THE DRAWINGS
[0035] Figure 1 It is the reaction route of fluorine-containing silicon-modified isocyanate. DETAILED DESCRIPTION
[0036] The specific embodiments of the present invention are described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the scope of the present invention.
[0037] In the embodiments, isophorone diisocyanate was purchased from BASF SE; polytetrahydrofuran diol was purchased from Hefei Tianjian Chemical Co., Ltd.; dibutyltin dilaurate and octadecyl methacrylate, azobisisobutylamidine hydrochloride, 2,3-dihydroxypropyl acrylate, 1,6-divinylperfluorohexane, and diethanolamine were all purchased from Aladdin Reagent Co., Ltd.; dimethylglyoxime was purchased from MacLean Biochemical Technology Co., Ltd.; and N-methyldiethanolamine was purchased from Alfa Aesar (China) Chemical Co., Ltd.
[0038] Example 1
[0039] (1) Under a nitrogen atmosphere, 1 mol of 1,6-divinylperfluorohexane and 10 mL of 1% chloroplatinic acid isopropanol solution were added to a flask, stirred and dispersed, and the temperature was raised to 125° C. 0.8 mol of heptamethyltrisiloxane was added thereto, and the reaction was stirred for 10 h. After the reaction was completed, the reaction was rotary evaporated to obtain intermediate 1.
[0040] (2) 0.5 mol of intermediate 1 and 0.75 mol of diethanolamine were added to 50 mL of isopropanol solvent, stirred and dispersed, heated to 75° C., and reacted for 1 h. After the reaction was completed, the intermediate 2 was washed with deionized water and dried to obtain the intermediate 2.
[0041] (3) 0.01 mol of intermediate 2 and 0.022 mol of isophorone diisocyanate were added to 50 mL of N,N-dimethylformamide solvent, stirred and mixed evenly, heated to 75° C., 0.08 mmol of dibutyltin dilaurate was added thereto, and the reaction was carried out for 3 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain fluorine-containing silicon-modified isocyanate.
[0042] (4) Under a nitrogen atmosphere, 0.1 mol of fluorinated silicon-modified isocyanate and 0.06 mol of polytetrahydrofuran diol were added to a flask, and the mixture was stirred at 80° C. for 2 h to obtain an isocyanate-terminated prepolymer.
[0043] (5) After the prepolymer is cooled to 45° C., 0.01 mol of MDEA and 0.2 mmol of DBTAL dissolved in 3 mL of acetone are added to extend the prepolymer chain to obtain a cationic prepolymer.
[0044] (6) 0.02 mol of GMMA dissolved in 5 mL of acetone was further added to the cationic prepolymer, the temperature was raised to 65° C. and the mixture was reacted for 2 hours, and then 0.01 mol of DMG dissolved in 3 mL of acetone was added and the reaction was continued for 2 hours to complete the chain extension reaction.
[0045] (7) The chain-extended prepolymer is cooled to room temperature and neutralized by adding 0.009 mol of acetic acid.
[0046] (8) Add 0.2 mol of SMA and slowly add 611 mL of deionized water under vigorous stirring to emulsify the mixture.
[0047] (9) The temperature was raised to 75° C., and 0.2 mmol of initiator AIBA dissolved in water was added dropwise to the emulsion and reacted for 6 hours. After the reaction was completed, a cationic hydrophobic treatment agent was obtained.
[0048] Example 2
[0049] (1) Under a nitrogen atmosphere, 1 mol of 1,6-divinylperfluorohexane and 10 mL of 1% by mass chloroplatinic acid isopropanol solution were added to a flask, stirred and dispersed, and the temperature was raised to 130° C. 1 mol of heptamethyltrisiloxane was added thereto, and the reaction was stirred for 6 h. After the reaction was completed, rotary evaporation was performed to obtain intermediate 1.
[0050] (2) 0.5 mol of intermediate 1 and 0.6 mol of diethanolamine were added to 50 mL of isopropanol solvent, stirred and dispersed, heated to 80° C., and reacted for 2 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain intermediate 2.
[0051] (3) 0.01 mol of intermediate 2 and 0.02 mol of isophorone diisocyanate were added to 50 mL of N,N-dimethylformamide solvent, stirred and mixed evenly, heated to 70° C., 0.1 mmol of dibutyltin dilaurate was added thereto, and the reaction was carried out for 6 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain fluorine-containing silicon-modified isocyanate.
[0052] (4) Under a nitrogen atmosphere, 0.1 mol of fluorinated silicon-modified isocyanate and 0.05 mol of polytetrahydrofuran diol were added to a flask, and the mixture was stirred at 80° C. for 2 h to obtain an isocyanate-terminated prepolymer.
[0053] (5) After the prepolymer is cooled to 45° C., 0.01 mol of MDEA and 0.2 mmol of DBTAL dissolved in 3 mL of acetone are added to extend the prepolymer chain to obtain a cationic prepolymer.
[0054] (6) 0.02 mol of GMMA dissolved in 5 mL of acetone was further added to the cationic prepolymer, the temperature was raised to 65° C. and the mixture was reacted for 2 hours, and then 0.02 mol of DMG dissolved in 3 mL of acetone was added and the reaction was continued for 2 hours to complete the chain extension reaction.
[0055] (7) The chain-extended prepolymer is cooled to room temperature and neutralized by adding 0.009 mol of acetic acid.
[0056] (8) Add 0.2 mol of SMA and slowly add 576 mL of deionized water under vigorous stirring to emulsify the mixture.
[0057] (9) The temperature was raised to 75° C., and 0.2 mol of initiator AIBA dissolved in water was added dropwise to the emulsion and reacted for 6 hours to obtain a cationic hydrophobic treatment agent.
[0058] Example 3
[0059] (1) Under a nitrogen atmosphere, 1 mol of 1,6-divinylperfluorohexane and 10 mL of 1% by mass chloroplatinic acid isopropanol solution were added to a flask, stirred and dispersed, and the temperature was raised to 120° C. 0.9 mol of heptamethyltrisiloxane was added thereto, and the reaction was stirred for 12 h. After the reaction was completed, rotary evaporation was performed to obtain intermediate 1.
[0060] (2) 0.5 mol of intermediate 1 and 0.5 mol of diethanolamine were added to 50 mL of isopropanol solvent, stirred and dispersed, heated to 82° C., and reacted for 3 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain intermediate 2.
[0061] (3) 0.01 mol of intermediate 2 and 0.24 mol of isophorone diisocyanate were added to 50 mL of N,N-dimethylformamide solvent, stirred and mixed evenly, heated to 80° C., 0.05 mmol of dibutyltin dilaurate was added thereto, and the reaction was carried out for 5 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain fluorine-containing silicon-modified isocyanate.
[0062] (4) Under a nitrogen atmosphere, 0.1 mol of fluorinated silicon-modified isocyanate and 0.05 mol of polytetrahydrofuran diol were added to a flask, and the mixture was stirred at 80° C. for 2 h to obtain an isocyanate-terminated prepolymer.
[0063] (5) After the prepolymer is cooled to 45° C., 0.01 mol of MDEA and 0.2 mol of DBTAL dissolved in 3 mL of acetone are added to extend the prepolymer chain to obtain a cationic prepolymer.
[0064] (6) 0.01 mol of GMMA dissolved in 3 mL of acetone was further added to the cationic prepolymer, the temperature was raised to 65° C. and the mixture was reacted for 2 hours, and then 0.02 mol of DMG dissolved in 3 mL of acetone was added and the reaction was continued for 2 hours to complete the chain extension reaction.
[0065] (7) The chain-extended prepolymer is cooled to room temperature and neutralized by adding 0.009 mol of acetic acid.
[0066] (8) Add 0.1 mol of SMA and slowly add 437 mL of deionized water under vigorous stirring to emulsify the mixture.
[0067] (9) The temperature was raised to 75° C., and 0.2 mmol of initiator AIBA dissolved in water was added dropwise to the emulsion and reacted for 6 hours to obtain a cationic hydrophobic treatment agent.
[0068] Example 4
[0069] (1) Under a nitrogen atmosphere, 1 mol of 1,6-divinylperfluorohexane and 10 mL of 1% chloroplatinic acid isopropanol solution were added to a flask, stirred and dispersed, and the temperature was raised to 130° C. 0.9 mol of heptamethyltrisiloxane was added thereto, and the reaction was stirred for 10 h. After the reaction was completed, the reaction was rotary evaporated to obtain intermediate 1.
[0070] (2) 0.5 mol of intermediate 1 and 0.6 mol of diethanolamine were added to 50 mL of isopropanol solvent, stirred and dispersed, heated to 78° C., and reacted for 2 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain intermediate 2.
[0071] (3) 0.01 mol of intermediate 2 and 0.022 mol of isophorone diisocyanate were added to 50 mL of N,N-dimethylformamide solvent, stirred and mixed evenly, heated to 75° C., 0.06 mmol of dibutyltin dilaurate was added thereto, and the reaction was carried out for 4 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain fluorine-containing silicon-modified isocyanate.
[0072] (4) Under a nitrogen atmosphere, 0.1 mol of fluorinated silicon-modified isocyanate and 0.04 mol of polytetrahydrofuran diol were added to a flask, and the mixture was stirred at 80° C. for 2 h to obtain an isocyanate-terminated prepolymer.
[0073] (5) After the prepolymer is cooled to 45° C., 0.01 mol of MDEA and 0.2 mol of DBTAL dissolved in 3 mL of acetone are added to extend the prepolymer chain to obtain a cationic prepolymer.
[0074] (6) 0.03 mol of GMMA dissolved in 8 mL of acetone was further added to the cationic prepolymer, the temperature was raised to 65° C. and the mixture was reacted for 2 hours, and then 0.02 mol of DMG dissolved in 5 mL of acetone was added and the reaction was continued for 2 hours to complete the chain extension reaction.
[0075] (7) The chain-extended prepolymer is cooled to room temperature and neutralized by adding 0.009 mol of acetic acid.
[0076] (8) Add 0.3 mol of SMA and slowly add 675 mL of deionized water under vigorous stirring to emulsify.
[0077] (9) The temperature was raised to 75° C., and 0.4 mmol of initiator AIBA dissolved in water was added dropwise to the emulsion. The reaction was allowed to proceed for 6 hours. After the reaction was completed, a cationic hydrophobic treatment agent was obtained.
[0078] Comparative Example 1
[0079] The difference between this comparative example and Example 1 is that 1,4-butanediol (BDO) is used instead of DMG.
[0080] Comparative Example 2
[0081] The difference between this comparative example and Example 1 is that BDO is used instead of MDEA.
[0082] Comparative Example 3
[0083] The difference between this comparative example and Example 1 is that BDO is used instead of GMMA.
[0084] Comparative Example 4
[0085] The difference between this comparative example and Example 1 is that isophorone diisocyanate is used instead of fluorine-containing silicon-modified isocyanate.
[0086] The cotton fabric is continuously immersed in a pre-impregnation cylinder filled with a hydrophobic treatment agent for pre-impregnation treatment. The pre-impregnation process time is 30 minutes and the pre-impregnation speed is 10m / min. Then it enters the impregnation machine for impregnation treatment. The rolling pressure is 50N and the impregnation speed is 10cm / min. Finally, the impregnation-treated fabric is baked at 160℃ for 2 minutes and cooled.
[0087] Water repellency test:
[0088] Test method: The hydrophobicity of the samples was measured at 25°C using a contact angle meter. The medium was deionized water. The water contact angles of each group of samples were tested at 5 different locations. The highest and lowest values were removed and the average of the remaining values was taken.
[0089] Table 1:
[0090] Contact angle before washing (°) 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 larger the contact angle, the better the hydrophobicity. It can be seen from the table that the water repellent prepared by the present invention has a good hydrophobic effect.
[0092] Flexibility test:
[0093] Test method: Press a 200g weight on the present embodiment at 25°C, remove the weight after 1 hour and observe the crease. To eliminate the error, press a 200g weight again in the vertical direction of the first crease, remove the weight after 1 hour and observe the crease.
[0094] Table 2
[0095] Crease performance Example 1 Not obvious Example 2 Not obvious Example 3 Not obvious Example 4 Not obvious Comparative Example 1 obvious Comparative Example 2 Not obvious Comparative Example 3 Not obvious Comparative Example 4 More obvious
[0096] It can be seen from the table that the hydrophobic treatment agent prepared by the present invention can improve the flexibility of cotton fabric after the cotton fabric is finished.
[0097] Emulsion stability test:
[0098] Test method: Use the oven method in GB / T 16497-2007, place 100 ml of the sample in a constant temperature oven at 85±1℃ for 48 hours, then let it stand at room temperature for 1 hour, and test the moisture content in the upper and lower samples according to the method specified in GB / T 11275-2007 to determine the stability of the emulsion.
[0099] Emulsion stability Example 1 Stablize Example 2 Stablize Example 3 Stablize Example 4 Stablize Comparative Example 1 Stablize Comparative Example 2 Stablize Comparative Example 3 Unstable Comparative Example 4 Unstable
[0100] It can be seen from the table that the hydrophobic treatment agent prepared by the present invention has good stability.
Claims
1. A cationic hydrophobic treatment agent for cotton fabrics, characterized in that: The hydrophobic treatment agent is a cationic waterborne polyurethane modified polyacrylate, comprising the following components in molar parts: 100 parts of fluorine-containing silicon-modified isocyanate, 40-60 parts of polytetramethylene glycol (PTMG), 10-20 parts of dynamic bond type chain extender, 30 parts of tertiary amine type chain extender, 10-30 parts of double bond type chain extender, 100-300 parts of octadecyl methacrylate (SMA), 0.2 parts of organotin catalyst, 0.2-0.5 parts of azobisisobutyramidine hydrochloride (AIBA); The molecular weight of the polytetrahydrofuran diol is M=1000 g / mol; The dynamic bond type chain extender is dimethylglyoxime (DMG); The tertiary amine chain extender is N-methyldiethanolamine (MDEA); The double bond type chain extender is 2,3-dihydroxypropyl acrylate (GMMA); The organotin 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, fluorine-containing silicon-modified isocyanate and polytetrahydrofuran diol are added to a flask, and stirred at 80° C. for 2 h to obtain an isocyanate-terminated prepolymer; (2) After cooling the prepolymer to 45° C., MDEA and DBTAL dissolved in acetone are added to achieve chain extension of the prepolymer to obtain a cationic prepolymer; (3) GMMA dissolved in acetone is continuously added to the cationic prepolymer, the temperature is raised to 65° C. and the reaction is continued for 2 hours, and then DMG dissolved in acetone is added and the reaction is continued for 2 hours to complete the chain extension reaction; (4) cooling the chain-extended prepolymer to room temperature and adding acetic acid for neutralization; (5) Add SMA and slowly add deionized water under vigorous stirring to emulsify; (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.
2. The cationic hydrophobic treatment agent for cotton fabric according to claim 1, characterized in that: In the step (2), the MDEA dissolved in acetone is prepared by dissolving 1 mass part of MDEA in 1-3 mass parts of acetone solvent.
3. The cationic hydrophobic treatment agent for cotton fabric according to claim 1, characterized in that: In the step (3), the GMMA dissolved in acetone is prepared by dissolving 1 mass part of GMMA in 1-3 mass parts of acetone solvent; and the DMG dissolved in acetone is prepared by dissolving 1 mass part of DMG in 1-3 mass parts of acetone solvent.
4. The cationic hydrophobic treatment agent for cotton fabric according to claim 1, characterized in that: The preparation method of the fluorine-containing silicon-modified isocyanate is as follows: A1. Under a nitrogen atmosphere, add 1,6-divinylperfluorohexane and 1% by mass chloroplatinic acid isopropanol solution into a flask, stir and disperse, heat to 120-130° C., add heptamethyltrisiloxane, stir and react for 6-12 hours, and after the reaction is completed, rotary evaporate to obtain intermediate 1; A2, adding intermediate 1 and diethanolamine to isopropanol solvent, stirring and dispersing, heating to 75-82°C, reacting for 1-3h, washing with deionized water after the reaction, and drying to obtain intermediate 2; A3. Add intermediate 2 and isophorone diisocyanate to N,N-dimethylformamide solvent, stir and mix evenly, heat to 70-80°C, add dibutyltin dilaurate thereto, react for 3-6 hours, and after the reaction is completed, wash with deionized water and dry to obtain fluorine-containing silicon-modified isocyanate.
5. The cationic hydrophobic treatment agent for cotton fabric according to claim 4, characterized in that: In the A1, the molar ratio of 1,6-divinylperfluorohexane to heptamethyltrisiloxane is 1:0.8-1.
6. The cationic hydrophobic treatment agent for cotton fabric according to claim 4, characterized in that: In the A2, the molar ratio of the intermediate 1 to diethanolamine is 1:1-1.
5.
7. The cationic hydrophobic treatment agent for cotton fabric according to claim 4, characterized in that: In the A3, the molar ratio of the intermediate 2, isophorone diisocyanate and dibutyltin dilaurate is 1:2-2.4:0.005-0.01.
Citation Information
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