Organic silicon waterproof finishing agent and preparation method thereof

The silicone waterproof finishing agent is prepared by using non-ionic silicon-containing surfactants, which solves the problems of water-resistant performance and environmental hazards of waterproof agents, achieves the combination of high-efficiency waterproofing and soft feel, and is suitable for a variety of fiber materials.

CN120776591AActive Publication Date: 2025-10-14HANGZHOU YUECHUANG FUTURE NEW MATERIAL TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202511292515.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-11
Publication Date
2025-10-14
Estimated Expiration
2045-09-11

AI Technical Summary

Technical Problem

Existing waterproofing agents have deficiencies in water resistance and film-forming properties, and traditional fluorine-containing waterproofing agents have potential hazards to the environment, making it difficult to meet the high-end market's demand for waterproof performance and feel.

Method used

By using non-ionic silicon-containing surfactants, the amount of organosilicon compounds is reduced to 5-10%. By synthesizing side-chain hydrogenated silicone oil, modified silicone oil and amino-modified silicone oil, and combining the emulsification process, an organosilicon waterproof finishing agent is prepared to form a three-dimensional network structure to improve washability and soft feel.

Benefits of technology

It achieves high wash resistance and excellent waterproof effect, while giving the fabric a soft feel, reducing raw material costs and avoiding environmental harm, and is suitable for a variety of fiber materials.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the field of textile functional finishing agents, in particular to an organosilicon waterproof finishing agent and a preparation method thereof.The preparation method comprises the steps that octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and an initiator are mixed to react, and side chain hydrogen-containing silicone oil is obtained through filtering; the preparation method comprises the following steps: mixing side chain hydrogen-containing silicone oil with 4-vinyl epoxy cyclohexane and a methacrylate compound, reacting under the protection of nitrogen, and adding a catalyst to obtain modified silicone oil; mixing and reacting the modified silicone oil with a coupling agent to obtain amino modified silicone oil; the preparation method comprises the following steps: mixing side chain hydrogen-containing silicone oil with allyl polyethylene glycol for reaction to obtain a nonionic silicon-containing surfactant; and finally, mixing the amino modified silicone oil with a nonionic silicon-containing surfactant, adding an acid solution, and adding water for emulsification to obtain the organosilicon waterproof finishing agent. Through the specific modified silicone oil and the nonionic silicon-containing surfactant, a uniform and stable waterproof film is formed on the surface of the fabric, the waterproof grade is improved, and the waterproof finishing agent is suitable for waterproof finishing of various fabrics.
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Description

Technical Field

[0001] The present invention relates to the field of functional finishing agents for textiles, and in particular to an organosilicon waterproof finishing agent and a preparation method thereof. Background Art

[0002] With the continuous development of the textile industry, demands for fabric waterproofing and a superior feel are increasing. Traditional waterproofing agents are primarily categorized into two main groups: fluorine-containing and fluorine-free. Fluorine-containing waterproofing agents are widely used for their excellent waterproofing properties, but their environmental impact has drawn widespread attention. Fluorine-containing waterproofing agents are primarily categorized into two types: C8 and C6. While C8 offers superior waterproofing performance, it is being phased out of the market due to its potential environmental hazards. C6 offers relatively weak waterproofing properties and struggles to achieve optimal waterproofing on some specialty fabrics.

[0003] Fluorine-free waterproofing agents primarily include acrylic and polyurethane. While environmentally friendly, acrylic waterproofing agents offer limited waterproofing effectiveness and leave a stiff feel on the finished fabric, making them difficult to meet the demands of the high-end market. Polyurethane waterproofing agents offer better waterproofing, but they suffer from poor air permeability, are prone to heat buildup, are expensive, and are prone to scratches, limiting their application.

[0004] Furthermore, existing waterproofing agents also have shortcomings in terms of washability and film-forming properties. Many waterproofing agents significantly reduce their effectiveness after repeated washing, failing to meet consumer demand for durable waterproofing. Furthermore, some waterproofing agents also exhibit poor film-forming properties on fabric surfaces, affecting the appearance and feel of the fabric. Summary of the Invention

[0005] In order to solve the problems in the background technology, the present invention proposes a silicone waterproof finishing agent and a preparation method thereof, which uses a non-ionic silicon-containing surfactant, and the dosage is only 5-10% of the silicone compound. Compared with the ordinary non-ionic surfactant dosage of generally 30-50% of the silicone compound, it not only reduces the raw material cost, but also reduces the negative impact of surfactant residue on waterproof performance.

[0006] The technical solution adopted by the present invention to solve the technical problem is: to provide a preparation method of an organic silicon waterproof finishing agent, comprising the following steps: S1, synthesizing side chain hydrogen-containing silicone oil: mixing octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane with a first catalyst, reacting at a set temperature and then filtering to obtain side chain hydrogen-containing silicone oil; S2, synthesizing modified silicone oil: mixing the side chain hydrogen-containing silicone oil obtained in S1, 4-vinyl cyclohexene oxide and a methacrylate compound, reacting under nitrogen protection, and adding a second Catalyst to obtain modified silicone oil; S3, synthesis of amino-modified silicone oil: the modified silicone oil obtained in S2 is mixed with a coupling agent, and the mixture is reacted at a set temperature to obtain amino-modified silicone oil; S4, preparation of non-ionic silicon-containing surfactant: the side-chain hydrogen-containing silicone oil obtained in S1 is mixed with allyl polyethylene glycol, and the mixture is reacted under nitrogen protection to obtain a non-ionic silicon-containing surfactant; S5, emulsification: the amino-modified silicone oil obtained in S3 is mixed with the non-ionic silicon-containing surfactant obtained in S4, an acid solution is added, and water is added for emulsification to obtain a silicone waterproof finishing agent.

[0007] Furthermore, in step S1, the mass ratio of octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane to the initiator is 100:(1-2):(2-20):(3-5); and the first catalyst is a solid acid resin.

[0008] Furthermore, the reaction temperature of step S1 is 50-70° C., and the reaction time is 6-8 hours.

[0009] Furthermore, in step S2, the molar ratio of side chain hydrogen silicone oil, 4-vinyl cyclohexene oxide, and methacrylate compound is 1:(4-20):(2-5); the reaction temperature is 80-100° C., and the reaction time is 4-6 hours; and the second catalyst is chloroplatinic acid.

[0010] Furthermore, the methacrylate compound is selected from lauryl methacrylate, tetradecyl methacrylate, hexadecyl methacrylate or octadecyl methacrylate.

[0011] Furthermore, 4-vinylcyclohexene oxide can be replaced by allyl glycidyl ether.

[0012] Furthermore, in step S3, the coupling agent is selected from 3-aminopropyltriethoxysilane, N-(2-aminoethyl-3-aminopropyl)methyldimethoxysilane or 3-aminopropylmethyldiethoxysilane; the molar ratio of modified silicone oil to coupling agent is 1:(1.5-3); the coupling agent is added dropwise for 1-1.5 hours; the reaction temperature is 50-70°C, and the reaction time is 4-6 hours.

[0013] Furthermore, in step S4, the molecular weight of the allyl polyethylene glycol is 580-700; the reaction temperature is 80-100° C., and the reaction time is 4-6 hours.

[0014] Furthermore, in step S5, the acid solution is an 80% acetic acid solution; the mass ratio of the amino-modified silicone oil, the nonionic silicon-containing surfactant and the 80% acetic acid solution is 100:(5-10):(1.2-1.5).

[0015] Furthermore, a silicone waterproof finishing agent is provided, comprising: octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane, 4-vinylepoxycyclohexane, a methacrylate compound, a coupling agent, allyl polyethylene glycol, 80% acetic acid solution, a first catalyst, and a second catalyst.

[0016] The beneficial effects of the present invention are:

[0017] (1) The present invention uses a nonionic silicon-containing surfactant, the dosage of which is only 5-10% of the organosilicon compound. Compared with the conventional nonionic surfactant which is generally used at 30-50% of the organosilicon compound, the present invention not only reduces the raw material cost but also reduces the negative impact of the surfactant residue on the waterproof performance.

[0018] (2) The organosilicon waterproof finishing agent of the present invention does not contain fluorine compounds, thus avoiding the potential harm to the environment caused by traditional fluorine-containing waterproofing agents and conforming to current environmental protection trends and market demands.

[0019] (3) By retaining some active groups such as epoxy groups and not participating in the ring-opening reaction of amino groups, and by hydrolyzing ethoxy groups into hydroxyl groups and forming a network-like three-dimensional structure during high-temperature setting, the waterproof finishing agent of the present invention can still maintain good waterproof performance after multiple water washings, thereby significantly improving the water washing resistance.

[0020] (4) The silicone waterproof finishing agent of the present invention not only provides excellent waterproof performance but also gives the fabric a soft and comfortable feel. The introduction of amino-modified silicone oil improves the feel of the fabric, achieving a good balance between waterproofness and hand feel. DETAILED DESCRIPTION

[0021] The following will be combined with the embodiments of the invention to clearly and completely describe the technical solutions in the embodiments of the invention. It should be understood that the specific embodiments described herein are only used to illustrate the present invention and are not intended to limit the present invention. It should also be noted that for ease of description, only some of the structures related to the present invention are shown, not all of them.

[0022] Example 1: Step S1: Synthesis of side chain hydrogen-containing silicone oil.

[0023]

[0024] As shown in the above formula, octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and solid acid resin are mixed in a mass ratio of 100:1.5:10:4, added to a four-necked flask, heated to 60°C, stirred and reacted for 7 hours, and filtered after the reaction to obtain side chain hydrogen-containing silicone oil.

[0025] Step S2: synthesizing modified silicone oil.

[0026]

[0027] Among them, x≥1, y≥1, y≥a+b.

[0028] As shown in the above formula, 100 g of the side-chain hydrogenated silicone oil obtained in step S1, 4-vinylcyclohexene oxide, and octadecyl methacrylate were added to a three-necked flask, purged with nitrogen, and the temperature was raised to 90°C. Chloroplatinic acid catalyst was slowly added dropwise and allowed to react for 5 hours to obtain epoxy-methacrylate co-modified silicone oil. The molar ratio of the side-chain hydrogenated silicone oil, 4-vinylcyclohexene oxide, and methacrylate compound was 1:12:3.

[0029] Step S3: synthesizing amino-modified silicone oil.

[0030]

[0031] As shown in the above formula, the modified silicone oil obtained in step S2 was mixed with 3-aminopropyltriethoxysilane in a molar ratio of 1:2, the 3-aminopropyltriethoxysilane was added dropwise for 1.2 hours, and the mixture was reacted at 60° C. for 5 hours to obtain amino-modified silicone oil.

[0032] Step S4: preparing a nonionic silicon-containing surfactant.

[0033] 50 g of the side chain hydrogenated silicone oil obtained in step S1 and 30 g of allyl polyethylene glycol with a molecular weight of 600 were added to a reaction kettle, heated to 90° C. under nitrogen protection, and reacted for 5 hours to obtain a nonionic silicon-containing surfactant.

[0034] Step S5: emulsification.

[0035] 100 g of the amino-modified silicone oil obtained in step S3, 8 g of the nonionic silicon-containing surfactant obtained in step S4, and 1.3 g of 80% acetic acid solution were mixed and emulsified using a high-speed shear disperser at a speed of 4000 r / min. Water was slowly added to adjust the emulsion solid content to 30% to obtain a silicone waterproof finishing agent.

[0036] Example 2: Step S1: Synthesis of side chain hydrogen-containing silicone oil.

[0037] Octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and solid acid resin were mixed in a mass ratio of 100:1:15:3, added to a four-necked flask, heated to 55° C., stirred and reacted for 8 hours, and filtered after the reaction to obtain side chain hydrogen-containing silicone oil.

[0038] Step S2: synthesizing modified silicone oil.

[0039] 100 g of the side-chain hydrogenated silicone oil obtained in step S1, 4-vinylcyclohexene oxide, and hexadecyl methacrylate were added to a three-necked flask. A nitrogen atmosphere was introduced and the temperature was raised to 85°C. Chloroplatinic acid catalyst was slowly added dropwise and allowed to react for 6 hours to obtain epoxy-methacrylate co-modified silicone oil. The molar ratio of the side-chain hydrogenated silicone oil, 4-vinylcyclohexene oxide, and methacrylate compound was 1:8:4.

[0040] Step S3: synthesizing amino-modified silicone oil.

[0041] The modified silicone oil obtained in step S2 was mixed with N-(2-aminoethyl-3-aminopropyl)methyldimethoxysilane in a molar ratio of 1:2.5, the coupling agent was added dropwise for 1.5 hours, and the mixture was reacted at 65° C. for 4.5 hours to obtain amino-modified silicone oil.

[0042] Step S4: preparing a nonionic silicon-containing surfactant.

[0043] 60 g of the side chain hydrogenated silicone oil obtained in step S1 and 25 g of allyl polyethylene glycol with a molecular weight of 580 were added to a reaction kettle, heated to 85° C. under nitrogen protection, and reacted for 6 hours to obtain a nonionic silicon-containing surfactant.

[0044] Step S5: emulsification.

[0045] 100 g of the amino-modified silicone oil obtained in step S3, 10 g of the nonionic silicon-containing surfactant obtained in step S4, and 1.5 g of 80% acetic acid solution were mixed and emulsified using a high-speed shear disperser at a speed of 3500 r / min. Water was slowly added to adjust the emulsion solid content to 30% to obtain a silicone waterproof finishing agent.

[0046] Example 3: Step S1: Synthesis of side chain hydrogen-containing silicone oil.

[0047] Octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and solid acid resin were mixed in a mass ratio of 100:2:5:5, added to a four-necked flask, heated to 70°C, stirred and reacted for 6 hours, and filtered after the reaction to obtain side chain hydrogen-containing silicone oil.

[0048] Step S2: synthesizing modified silicone oil.

[0049] 100 g of the side-chain hydrogenated silicone oil obtained in step S1, allyl glycidyl ether, and lauryl methacrylate were added to a three-necked flask. Nitrogen was introduced and the temperature was raised to 100°C. Chloroplatinic acid catalyst was slowly added dropwise and allowed to react for 4 hours to obtain epoxy-methacrylate co-modified silicone oil. The molar ratio of the side-chain hydrogenated silicone oil, allyl glycidyl ether, and methacrylate compound was 1:20:2.

[0050] Step S3: synthesizing amino-modified silicone oil.

[0051] The modified silicone oil obtained in step S2 was mixed with 3-aminopropylmethyldiethoxysilane (KH-912) in a molar ratio of 1:1.8, the coupling agent was added dropwise for 1 hour, and the mixture was reacted at 70°C for 5.5 hours to obtain amino-modified silicone oil.

[0052] Step S4: preparing a nonionic silicon-containing surfactant.

[0053] 40 g of the side chain hydrogenated silicone oil obtained in step S1 and 35 g of allyl polyethylene glycol with a molecular weight of 700 were added to a reaction kettle, heated to 100° C. under nitrogen protection, and reacted for 4 hours to obtain a nonionic silicon-containing surfactant.

[0054] Step S5: emulsification.

[0055] 100 g of the amino-modified silicone oil obtained in step S3, 5 g of the nonionic silicon-containing surfactant obtained in step S4, 1.2 g of 80% acetic acid solution, and 210 g of water were mixed, and emulsified for 2 hours using a high-speed shear disperser at a speed of 4500 r / min. Water was slowly added to adjust the emulsion solid content to 30% to obtain a silicone waterproof finishing agent.

[0056] Example 4: Step S1: Synthesis of side chain hydrogen-containing silicone oil.

[0057] Octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and solid acid resin were mixed in a mass ratio of 100:1.8:18:3.5, added to a four-necked flask, heated to 65° C., stirred and reacted for 7.5 hours, and filtered after the reaction to obtain side chain hydrogen-containing silicone oil.

[0058] Step S2: Synthesis of modified silicone oil

[0059] Add 100g of the side-chain hydrogenated silicone oil obtained in step S1, 4-vinylcyclohexene oxide, and tetradecyl methacrylate to a three-necked flask. Pour nitrogen into the flask, raise the temperature to 95°C, and slowly add chloroplatinic acid as a catalyst. Allow to react for 5.5 hours to obtain epoxy-methacrylate co-modified silicone oil. The molar ratio of the side-chain hydrogenated silicone oil, 4-vinylcyclohexene oxide, and methacrylate compound is 1:15:3.5.

[0060] Step S3: synthesizing amino-modified silicone oil.

[0061] The modified silicone oil obtained in step S2 was mixed with 3-aminopropyltriethoxysilane in a molar ratio of 1:2.2, the coupling agent was added dropwise for 1.3 hours, and the mixture was reacted at 55° C. for 6 hours to obtain amino-modified silicone oil.

[0062] Step S4: preparing a nonionic silicon-containing surfactant.

[0063] 55 g of the side chain hydrogenated silicone oil obtained in step S1 and 28 g of allyl polyethylene glycol with a molecular weight of 650 were added to a reaction kettle. The temperature was raised to 95° C. under nitrogen protection and the reaction was carried out for 5.5 hours to obtain a nonionic silicon-containing surfactant.

[0064] Step S5: emulsification.

[0065] Mix 100 g of the amino-modified silicone oil obtained in step S3, 7 g of the nonionic silicon-containing surfactant obtained in step S4, 1.4 g of an 80% acetic acid solution, and 240 g of water. Emulsify the mixture using a high-speed shear disperser at 3800 r / min for 2.2 hours. Slowly add water to adjust the emulsion solids content to 30%, to obtain a silicone waterproofing finish.

[0066] Example 5: Step S1: Synthesis of side chain hydrogen-containing silicone oil.

[0067] Octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and solid acid resin were mixed in a mass ratio of 100:1.2:8:4.5, added to a four-necked flask, heated to 58° C., stirred and reacted for 8 hours, and filtered after the reaction to obtain side chain hydrogen-containing silicone oil.

[0068] Step S2: synthesizing modified silicone oil.

[0069] Add 100g of the side-chain hydrogenated silicone oil obtained in step S1, 4-vinylcyclohexene oxide, and octadecyl methacrylate to a three-necked flask. Pour nitrogen into the flask, raise the temperature to 88°C, and slowly add chloroplatinic acid as a catalyst. Allow to react for 5.5 hours to obtain epoxy-methacrylate co-modified silicone oil. The molar ratio of the side-chain hydrogenated silicone oil, 4-vinylcyclohexene oxide, and methacrylate compound is 1:18:4.5.

[0070] Step S3: synthesizing amino-modified silicone oil.

[0071] The modified silicone oil obtained in step S2 was mixed with 3-aminopropylmethyldiethoxysilane in a molar ratio of 1:2.8, the coupling agent was added dropwise for 1.4 hours, and the mixture was reacted at 68° C. for 4.8 hours to obtain amino-modified silicone oil.

[0072] Step S4: preparing a nonionic silicon-containing surfactant.

[0073] 48 g of the side chain hydrogenated silicone oil obtained in step S1 and 32 g of allyl polyethylene glycol with a molecular weight of 680 were added to a reaction kettle, heated to 92° C. under nitrogen protection, and reacted for 4.8 hours to obtain a nonionic silicon-containing surfactant.

[0074] Step S5: emulsification.

[0075] 100 g of the amino-modified silicone oil obtained in step S3, 9 g of the nonionic silicon-containing surfactant obtained in step S4, 1.1 g of 80% acetic acid solution, and 220 g of water were mixed, and emulsified for 2.3 hours using a high-speed shear disperser at a speed of 4200 r / min. Water was slowly added to adjust the emulsion solid content to 30% to obtain a silicone waterproof finishing agent.

[0076] Example 6: Step S1: Synthesis of side chain hydrogen-containing silicone oil.

[0077] Octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane, and solid acid resin were mixed in a mass ratio of 100:1.7:12:3.8 and added to a four-necked flask. The mixture was heated to 62°C and stirred for 7.2 hours. After the reaction was complete, the mixture was filtered to obtain a side-chain hydrogenated silicone oil.

[0078] Step S2: synthesizing modified silicone oil.

[0079] 100g of the side-chain hydrogenated silicone oil obtained in step S1, allyl glycidyl ether, and hexadecyl methacrylate were added to a three-necked flask. A nitrogen atmosphere was introduced, and the temperature was raised to 93°C. Chloroplatinic acid catalyst (0.05% of the total mass) was slowly added dropwise. The reaction was allowed to proceed for 5.2 hours to obtain epoxy-methacrylate co-modified silicone oil. The molar ratio of the side-chain hydrogenated silicone oil, allyl glycidyl ether, and methacrylate compound was 1:10:4.

[0080] Step S3: synthesizing amino-modified silicone oil.

[0081] The modified silicone oil obtained in step S2 was mixed with N-(2-aminoethyl-3-aminopropyl)methyldimethoxysilane in a molar ratio of 1:2.3, the coupling agent was added dropwise for 1.1 hours, and the mixture was reacted at 63° C. for 5.8 hours to obtain amino-modified silicone oil.

[0082] Step S4: preparing a nonionic silicon-containing surfactant.

[0083] 53 g of the side chain hydrogenated silicone oil obtained in step S1 and 29 g of allyl polyethylene glycol with a molecular weight of 620 were added to a reaction kettle, heated to 87° C. under nitrogen protection, and reacted for 5.3 hours to obtain a nonionic silicon-containing surfactant.

[0084] Step S5: emulsification.

[0085] 100 g of the amino-modified silicone oil obtained in step S3, 6 g of the nonionic silicon-containing surfactant obtained in step S4, 1.3 g of 80% acetic acid solution, and 235 g of water were mixed, and emulsified for 2.1 hours using a high-speed shear disperser at a speed of 3900 r / min. Water was slowly added to adjust the emulsion solid content to 30%, thereby obtaining a silicone waterproof finishing agent.

[0086] Performance test example:

[0087] (1) Water repellency test method:

[0088] Refer to AATCC 22-2005, "Water Repellency Test: Spray Method," for the following test method: Take a treated fabric sample, clamp it tightly with a clamp, and position it at a 45° angle, with the warp direction of the fabric aligned with the direction of water droplets flowing down the fabric. Position the center of the test surface 15 cm below the center of the nozzle. Apply spray to the fabric surface over a period of 25-30 seconds. After spraying, remove the clamp and lay the fabric horizontally. Then, evaluate the test fabric against the rating criteria.

[0089] (2) Hand feel test method

[0090] A group of 5-8 people closed their eyes and touched the treated cotton fabric to compare its softness, scoring 1-5 points. The test was conducted three times on average and the average value was selected.

[0091]

[0092] The organosilicon waterproof finishing agent provided by the present invention shows excellent performance advantages in performance tests. The organosilicon waterproof finishing agent can achieve excellent initial waterproof effect at a dosage of 30 grams per liter on cotton fabrics and 10 grams per liter on polyester fabrics, with a water repellency score of more than 83 points, of which the initial water repellency of polyester fabrics is as high as 92 points, exceeding the level of conventional fluorine-free waterproofing agents; at the same time, it has water washability. After 10 washes, the water repellency of cotton fabrics is still stable at more than 73 points, up to 77 points, and the polyester fabric remains above 85 points, up to 87 points, effectively solving the pain point of insufficient durability of traditional waterproofing agents. While giving the fabric high-grade waterproof performance, the finishing agent makes the fabric feel soft and comfortable after finishing through the synergistic effect of amino-modified silicone oil. The cotton fabric feel score generally reaches more than 4 points, successfully overcoming the problem of hard feel caused by polyurethane waterproofing agents. In addition, this technology has a wide range of fiber applicability and can achieve efficient waterproofing at lower application concentrations, significantly reducing processing costs; its environmental protection characteristics are particularly outstanding. Through the innovative use of silicone-containing surfactants, the dosage is only 5% to 10% of organic silicon compounds, which is far lower than the 30% to 50% of conventional surfactants. It not only reduces the cost of raw materials and residual effects, but also does not contain fluorine compounds throughout the process, avoiding the environmental risks of fluorine-containing waterproofing agents, providing a solution that combines high performance and sustainability for the development of green textiles.

[0093] The present invention has been described in detail above with reference to the embodiments and comparative examples. However, the present invention is not limited to the above embodiments. Various modifications can be made within the scope of knowledge possessed by those skilled in the art without departing from the spirit of the present invention. Any content not described in detail in the present invention may be adapted from existing technologies.

Claims

1. A method for preparing an organosilicon waterproof finishing agent, characterized in that: The following steps are involved: S1. Synthesis of side chain hydrogen-containing silicone oil: octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane and a first catalyst are mixed, reacted at a set temperature and then filtered to obtain side chain hydrogen-containing silicone oil; S2. Synthesis of modified silicone oil: The side chain hydrogenated silicone oil obtained in S1, 4-vinyl cyclohexene oxide, and a methacrylate compound are mixed, reacted under nitrogen protection, and a second catalyst is added to obtain modified silicone oil; S3, synthesizing amino-modified silicone oil: mixing the modified silicone oil obtained in S2 with a coupling agent, and reacting at a set temperature to obtain amino-modified silicone oil; S4, preparing a nonionic silicon-containing surfactant: mixing the side chain hydrogen-containing silicone oil obtained in S1 with allyl polyethylene glycol, and reacting them under nitrogen protection to obtain a nonionic silicon-containing surfactant; S5. Emulsification: Mix the amino-modified silicone oil obtained in S3 and the nonionic silicon-containing surfactant obtained in S4, add the acid solution and emulsify with water to obtain a silicone waterproof finishing agent.

2. A method for preparing an organosilicon waterproof finishing agent according to claim 1, characterized in that: In step S1, the mass ratio of octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane to the initiator is 100:(1-2):(2-20):(3-5); and the first catalyst is a solid acid resin.

3. The method for preparing a silicone waterproof finishing agent according to claim 2, characterized in that: The reaction temperature of step S1 is 50-70° C., and the reaction time is 6-8 hours.

4. The method for preparing a silicone waterproof finishing agent according to claim 1, wherein: In step S2, the molar ratio of side chain hydrogen silicone oil, 4-vinyl cyclohexene oxide, and methacrylate compound is 1:(4-20):(2-5); the reaction temperature is 80-100° C., and the reaction time is 4-6 hours; and the second catalyst is chloroplatinic acid.

5. A method for preparing an organosilicon waterproof finishing agent according to claim 4, characterized in that: The methacrylate compounds include lauryl methacrylate, tetradecyl methacrylate, hexadecyl methacrylate or octadecyl methacrylate.

6. A method for preparing an organosilicon waterproof finishing agent according to claim 5, characterized in that: 4-Vinylcyclohexene oxide can be replaced by allyl glycidyl ether.

7. A method for preparing an organosilicon waterproof finishing agent according to claim 1, characterized in that: In step S3, the coupling agent includes 3-aminopropyltriethoxysilane, N-(2-aminoethyl-3-aminopropyl)methyldimethoxysilane or 3-aminopropylmethyldiethoxysilane; the molar ratio of modified silicone oil to coupling agent is 1:(1.5-3); the coupling agent is added dropwise for 1-1.5 hours; the reaction temperature is 50-70°C, and the reaction time is 4-6 hours.

8. A method for preparing an organosilicon waterproof finishing agent according to claim 1, characterized in that: In step S4, the molecular weight of the allyl polyethylene glycol is 580-700; the reaction temperature is 80-100° C., and the reaction time is 4-6 hours.

9. A method for preparing an organosilicon waterproof finishing agent according to claim 1, characterized in that: In step S5, the acid solution is an 80% acetic acid solution; the mass ratio of the amino-modified silicone oil, the nonionic silicon-containing surfactant, and the 80% acetic acid solution is 100:(5-10):(1.2-1.5).

10. An organosilicon waterproof finishing agent prepared by the preparation method of an organosilicon waterproof finishing agent according to any one of claims 1 to 9, characterized in that: include: Octamethylcyclotetrasiloxane, hexamethyldisiloxane, tetramethylcyclotetrasiloxane, 4-vinylcyclohexene oxide, methacrylate compound, coupling agent, allyl polyethylene glycol, 80% acetic acid solution, a first catalyst and a second catalyst.

Citation Information

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