Softening agent used together with waterproof agent in one bath as well as preparation method and application of softening agent
By preparing a softener, the problem of combining waterproofing agent and softener in the same bath is solved, and the efficient hydrophobic and soft effect of the fabric is achieved, and it is suitable for a variety of fabric materials.
Patent Information
- Application Number
- CN202510603006.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-12
- Publication Date
- 2025-07-29
- Estimated Expiration
- 2045-05-12
AI Technical Summary
The prior art is difficult to effectively combine waterproofing agents and softeners in the same bath method, resulting in a decrease in the waterproofing effect of the fabric or insufficient softness, and it is difficult to achieve stable compounding on different fabric materials.
Using a softener preparation method, a first intermediate is prepared by reacting double-ended hydrogen-containing silicone oil with long-chain carboene under the action of inert gas and catalyst, and then reacting with octamethylcyclotetrasiloxane, 3-methacryloyloxypropylmethyldimethoxysilane and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane, and finally reacting with organic diamine to prepare a softener used in the same bath as the waterproofing agent, and long-chain alkanes and silane segments of specific structures are introduced to improve compatibility and film formation.
It maintains the hydrophobic properties and softness of the fabric during use in the same bath, reduces the impact of waterproofing agent on the softener, improves the waterproofing level and wear comfort of the fabric, and is suitable for a variety of fabric materials.
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Abstract
Description
Technical Field
[0001] The present application relates to the field of polymer materials, and particularly to a softener for use in the same bath as a waterproofing agent, a preparation method thereof, and an application thereof. Background Art
[0002] With the continuous growth of the market demand for functional textiles such as outdoor sportswear, medical protective clothing, and home textiles, the demand for composite functional fabrics with waterproof, soft, and durable properties has increased sharply. Traditional single-functional finishing technologies can no longer meet the needs of high-end consumption and industrial applications. In traditional textile post-finishing processes, the waterproof and soft functions need to be achieved step by step using a two-bath method, that is, first perform waterproof treatment and then perform soft treatment. This process has problems such as complex processes, long processing cycles, large amounts of wastewater discharge, and high production costs. In addition, there are ionic conflicts between waterproofing agents and softeners. For example, when a cationic waterproofing agent is mixed with an anionic softener, it is easy to cause a decrease in product performance, making it difficult to simultaneously achieve both waterproofness and softness.
[0003] In recent years, the auxiliary formulation technology has been continuously innovated. The application of C6 waterproofing agents and the optimization of the compatibility of non-ionic / cationic softeners, combined with the application of nanotechnology, have made it possible to achieve the waterproof and soft functions synergistically in one bath. By reasonably compounding softeners and waterproofing agents, the one-bath process can significantly reduce water consumption, energy consumption, and chemical usage, promoting the transformation of the textile industry towards green and low-energy directions, which is in line with the concept of sustainable development.
[0004] Currently, products on the market that can be effectively compounded with waterproofing agents, have little impact on the waterproof effect, and can improve the hand feeling of fabrics after waterproof finishing are scarce. When most softeners are mixed with waterproofing agents, due to problems such as differences in chemical structure and ionic property conflicts, the hydrophobic effect of the waterproofing agent is significantly weakened, resulting in the fabric's waterproof grade not reaching the expected standard. Even some products can ensure the waterproof performance, but it is difficult to effectively improve the hard and rough touch problems of fabrics after waterproof finishing, seriously affecting the wearing comfort and product added value. In addition, limited by the existing technical level, products that meet the requirements of industrial large-scale production and can achieve stable compounding effects on different fabric materials (such as cotton, polyester fiber, nylon, etc.) are extremely rare. Therefore, products that can break through the above technical barriers, be effectively compounded with waterproofing agents, have little impact on the waterproof effect, and can significantly improve the hand feeling of fabrics after waterproof finishing are in short supply on the market and urgently need innovative technologies to fill the gap in this field. Summary of the Invention
[0005] The purpose of the present application is to provide a softener for use in the same bath as a waterproofing agent, which can improve the softness of fabrics while maintaining a good waterproof effect.
[0006] To achieve the above object, the technical solution adopted in this application is as follows: This application provides a softener for use in the same bath as a waterproofing agent, and its structural general formula is: Where m, x, y, z, and a are integers, and 9 ≤ m ≤ 13; 2 ≤ a ≤ 6; 291 ≤ x ≤ 374; 2 ≤ y ≤ 4; 3 ≤ z ≤ 5.
[0007] This application also provides a preparation method for a softener for use in the same bath as a waterproofing agent, including the following steps: S1: React a hydrogen-terminated polydimethylsiloxane with a long-chain alkene under the action of an inert gas and a catalyst to prepare a first intermediate; S2: React the first intermediate, octamethylcyclotetrasiloxane, 3-methacryloxypropylmethyldimethoxysilane, and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane to prepare a second intermediate; S3: React the second intermediate with an organic diamine to prepare the softener for use in the same bath as the waterproofing agent.
[0008] As a preference, the structural formula of the first intermediate is: Where m and n are integers, and 9 ≤ m ≤ 13; 27 ≤ n ≤ 40.
[0009] As another preference, the structural formula of the second intermediate is: Where m, n, x, y, and z are integers, and 9 ≤ m ≤ 13; 27 ≤ n ≤ 40; 291 ≤ x ≤ 374; 2 ≤ y ≤ 4; 3 ≤ z ≤ 5.
[0010] As another preference, by mass, the specific operation of step S1 is: Place 2000 - 3000 parts of the hydrogen-terminated polydimethylsiloxane and 336 - 448 parts of the long-chain alkene in a reaction vessel, heat up and add a catalyst under an inert gas atmosphere, and obtain the first intermediate after holding for a period of time.
[0011] As another preference, by mass, the specific operation of step S2 is: Place 2336 - 3448 parts of the first intermediate, 20540 - 27660 parts of octamethylcyclotetrasiloxane, 464 - 928 parts of 3-methacryloxypropylmethyldimethoxysilane, and 660 - 1100 parts of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane in a reaction vessel, add 1.3 - 1.5 parts of tetramethylammonium hydroxide and heat up, hold for a period of time and then continue to heat up, hold again for a period of time, and remove low-boiling substances under vacuum to obtain the second intermediate.
[0012] As another preference, by mass parts, the step S3 specifically is: putting 2500-3300 parts of the second intermediate, 18-58 parts of organic diamine and 2518-3358 parts of solvent into a reaction vessel, heating and keeping warm for a period of time, adding an initiator, and obtaining the softener used in the same bath as the waterproofing agent.
[0013] As another preference, the number of carbon atoms in the straight-chain main chain of the long-chain carbene is greater than or equal to 10.
[0014] Further preferably, the number-average molecular weight of the hydrogen-containing silicone oil at both ends is 2000-5000.
[0015] The present application also provides a softener product used in the same bath as the waterproofing agent, including the following raw materials by mass parts: 150-250 parts of water, 2-10 parts of emulsifier, 1-5 parts of glacial acetic acid, and 90-110 parts of the softener used in the same bath as the waterproofing agent as described in claim 1 or the softener used in the same bath as the waterproofing agent prepared by the preparation method as described in claims 2-9.
[0016] Compared with the prior art, the beneficial effects of the present application are as follows:
[0017] (1) For the softener used in the same bath as the waterproofing agent in the present application, a long-chain alkane is introduced into the structure, which acts together with the polysiloxane chain segment in the structure, has the effect of reducing the surface tension of the product, and can improve the hydrophobic property of the fabric surface after treating the fabric.
[0018] (2) For the softener used in the same bath as the waterproofing agent in the present application, a 3-methacryloxypropylmethyldimethoxysilane structural chain segment is introduced. The ester group can improve the compatibility between the softener product and the waterproofing agent; at the same time, in the presence of an initiator, the methacryloyl group can undergo a certain polymerization reaction after high-temperature setting, and together with the polysiloxane, it can endow the treated fabric with film-forming property, thereby reducing the influence of the waterproofing agent on the softener.
[0019] (3) For the softener used in the same bath as the waterproofing agent in the present application, when treating the fabric, the polysiloxane and amino group in the structure form a directional adsorption on the fabric surface, which can endow the fabric with excellent hand feeling and reduce the weakening effect on the hand feeling when the softener and the waterproofing agent are in the same bath. Specific embodiments
[0020] Next, in combination with specific embodiments, the present application will be further described. It should be noted that on the premise of no conflict, the following-described embodiments or technical features can be combined arbitrarily to form new embodiments.
[0021] The terms "comprising" and "having" in the description and claims of this application, and any variations thereof, are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or device that comprises a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units not clearly listed or inherent to these processes, methods, products, or devices.
[0022] This application provides a softener for use in the same bath as a waterproofing agent, and its structural general formula is: Where m, x, y, z, and a are integers, and 9 ≤ m ≤ 13; 2 ≤ a ≤ 6; 291 ≤ x ≤ 374; 2 ≤ y ≤ 4; 3 ≤ z ≤ 5.
[0023] The softener for use in the same bath as the waterproofing agent in this application introduces long-chain alkanes into its structure, which act together with the polysiloxane chain segments in the structure, having the effect of reducing the surface tension of the product and being able to improve the hydrophobic performance of the fabric surface after treating the fabric.
[0024] The softener for use in the same bath as the waterproofing agent in this application introduces a 3-methacryloxypropylmethyldimethoxysilane structural chain segment. The ester group can improve the compatibility of the softener product with the waterproofing agent. At the same time, in the presence of an initiator, the methacryloyl group can undergo a certain polymerization reaction after high-temperature setting, and together with the polysiloxane, it can endow the treated fabric with film-forming properties, thereby reducing the influence of the waterproofing agent on the softener.
[0025] When the softener for use in the same bath as the waterproofing agent in this application treats the fabric, the polysiloxane and amino groups in the structure form a directional adsorption on the fabric surface, which can endow the fabric with excellent handfeel and reduce the weakening effect on the handfeel when the softener and the waterproofing agent are in the same bath.
[0026] This application also provides a preparation method for a softener for use in the same bath as a waterproofing agent, including the following steps:
[0027] S1: React hydrogen-terminated polydimethylsiloxane with long-chain alkene under the action of an inert gas and a catalyst to prepare a first intermediate;
[0028] S2: React the first intermediate, octamethylcyclotetrasiloxane, 3-methacryloxypropylmethyldimethoxysilane, and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane to prepare a second intermediate;
[0029] S3: React the second intermediate with an organic diamine to prepare the softener for use in the same bath as the waterproofing agent in this application.
[0030] Among them, the structural formula of the first intermediate is: Where m and n are integers, and 9 ≤ m ≤ 13; 27 ≤ n ≤ 40.
[0031] The structural formula of the second intermediate is as follows: Wherein m, n, x, y, z are integers, and 9 ≤ m ≤ 13; 27 ≤ n ≤ 40; 291 ≤ x ≤ 374; 2 ≤ y ≤ 4; 3 ≤ z ≤ 5.
[0032] In some embodiments, by mass parts, the S1 step is specifically as follows: Put 2000 - 3000 parts of hydrogen-containing silicone oil with two terminals and 336 - 448 parts of long-chain carbene into a reaction vessel, under an inert gas atmosphere, heat up and add a catalyst, and obtain a first intermediate after keeping warm for a period of time.
[0033] The reaction formula of the hydrogen-containing silicone oil with two terminals and the long-chain carbene in the S1 step is: Wherein m and n are integers, and 9 ≤ m ≤ 13; 27 ≤ n ≤ 40.
[0034] In preferred embodiments, the number of carbon atoms in the straight-chain main chain of the long-chain carbene is greater than or equal to 10.
[0035] In some embodiments, by mass parts, the S2 step is specifically as follows: Put 2336 - 3448 parts of the first intermediate, 20540 - 27660 parts of octamethylcyclotetrasiloxane, 464 - 928 parts of 3-methacryloxypropylmethyldimethoxysilane, and 660 - 1100 parts of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane into a reaction vessel, add 1.3 - 1.5 parts of tetramethylammonium hydroxide and heat up, keep warm for a period of time and then continue to heat up, keep warm again for a period of time, and remove low-boiling substances under vacuum to obtain the second intermediate.
[0036] In the S2 step, the reaction formula of the first intermediate, octamethylcyclotetrasiloxane, 3-methacryloxypropylmethyldimethoxysilane, and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane is: Wherein m, n, x, y, z are integers, and 9 ≤ m ≤ 13; 27 ≤ n ≤ 40; 291 ≤ x ≤ 374; 2 ≤ y ≤ 4; 3 ≤ z ≤ 5.
[0037] In some embodiments, by mass parts, the S3 step is specifically as follows: Put 2500 - 3300 parts of the second intermediate, 18 - 58 parts of organic diamine, and 2518 - 3358 parts of solvent into a reaction vessel, heat up and keep warm for a period of time, add an initiator, and obtain the softener of the present application for use in the same bath as the waterproof agent.
[0038] In the S3 step, the reaction formula of the second intermediate and the organic diamine is: Where m, x, y, z, and a are integers, and 9 ≤ m ≤ 13; 2 ≤ a ≤ 6; 291 ≤ x ≤ 374; 2 ≤ y ≤ 4; 3 ≤ z ≤ 5.
[0039] This technology uses the hydrosilylation reaction to introduce long-chain alkane structures as capping agents. The introduction of long-chain alkanes can effectively reduce the surface tension, thereby enhancing the hydrophobic properties of the product. The cleavage rearrangement of the siloxane segments is used to introduce 3-methacryloxypropylmethyldimethoxysilane into the product structure. The methacryloyl structure therein can undergo a certain polymerization reaction under the action of an initiator during high-temperature setting, improving the film-forming performance of the product on the fabric surface, and thus reducing the impact on the waterproof effect of the waterproof agent. The reaction between epoxy groups and amino groups is used to introduce amino groups into the product structure. The combined action of the polysiloxane segments and amino groups endows the product with excellent soft handfeel.
[0040] This application also provides a softener product for use in the same bath as a waterproof agent, including: the softener for use in the same bath as the waterproof agent of this application, emulsifier 1303, water, and glacial acetic acid.
[0041] Example 1
[0042] Prepare a softener for use in the same bath as a waterproof agent. By mass:
[0043] S1: Add 2000 parts of hydrogen-terminated polydimethylsiloxane with an average molecular weight of 2000 and 336 parts of 1-dodecene to a reaction kettle equipped with a thermometer, a stirrer, and a condensing reflux device. Charge nitrogen, heat up to 75 °C, add 0.6 part of Karstedt catalyst, continue to heat up to 110 °C, and keep warm for 6 hours to obtain the first intermediate.
[0044] S2: Add 2336 parts of the first intermediate, 21550 parts of octamethylcyclotetrasiloxane, 464 parts of 3-methacryloxypropylmethyldimethoxysilane, and 660 parts of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane to a reaction kettle equipped with a thermometer, a stirrer, and a condensing reflux device. Stir well, add 1.3 parts of tetramethylammonium hydroxide, heat up to 100 °C, keep warm for 10 hours, then heat up to 135 °C, keep warm for 1 hour, and under a vacuum of -0.09 Mpa, remove the low-boiling substances to obtain the second intermediate.
[0045] S3: Add 2500 parts of the second intermediate, 18 parts of ethylenediamine, and 2518 parts of isopropanol to a reaction kettle equipped with a thermometer, a stirrer, and a condensing reflux device. Stir well, heat up to 78 °C, keep warm for 6 hours, and add 0.2 part of azobisisobutyronitrile ethanol solution to prepare a softener for use in the same bath as the waterproof agent in Example 1 of this application.
[0046] Example 2
[0047] Adjust the number-average molecular weight of the hydrogen-containing silicone oil at step S1 to 3000, and correspondingly adjust the addition amount to 3000 parts by mass, and adjust the dosage of the Karstedt catalyst to 0.8 parts by mass;
[0048] Adjust the addition amount of the first intermediate at step S2 to 3336 parts by mass, and adjust the addition amount of octamethylcyclotetrasiloxane to 20540 parts by mass. Other preparation steps are the same as those in Example 1.
[0049] Example 3
[0050] Adjust the long-chain alkene in step S1 to 1-hexadecene, and adjust the addition amount to 448 parts by mass. After adding the Karstedt catalyst, heat up to 120 °C; adjust the addition amount of the first intermediate in step S2 to 2448 parts by mass, and adjust the addition amount of octamethylcyclotetrasiloxane to 21430 parts by mass. Other preparation steps are the same as those in Example 1.
[0051] Example 4
[0052] Adjust the addition amount of octamethylcyclotetrasiloxane in step S2 to 26430 parts by mass; adjust the addition amount of the second intermediate in S3 to 3000 parts by mass, and adjust the addition amount of the solvent isopropanol to 3018 parts by mass. Other preparation steps are the same as those in Example 3.
[0053] Example 5
[0054] Adjust the addition amount of 3-methacryloxypropylmethyldimethoxysilane in step S2 to 928 parts by mass; adjust the addition amount of the second intermediate in step S3 to 3046 parts by mass, and adjust the addition amount of the solvent isopropanol to 3064 parts by mass. Other preparation steps are the same as those in Example 4.
[0055] Example 6
[0056] Adjust the addition amount of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane in step S2 to 1100 parts by mass; adjust the addition amount of the second intermediate in step S3 to 3044 parts by mass, adjust the addition amount of ethylenediamine to 30 parts by mass, and adjust the addition amount of the solvent isopropanol to 3074 parts by mass. Other preparation steps are the same as those in Example 4.
[0057] Example 7
[0058] Adjust the addition amount of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane in Step S2 to 1100 parts by mass; adjust the addition amount of the second intermediate in Step S3 to 3090 parts by mass, the addition amount of ethylenediamine to 30 parts by mass, and the addition amount of the solvent isopropanol to 3120 parts by mass. Other preparation steps are the same as those in Example 5.
[0059] Example 8
[0060] Adjust the organic diamine in Step S3 to 37 parts by mass of propanediamine, and adjust the addition amount of the solvent isopropanol to 3127 parts by mass. Other preparation steps are the same as those in Example 7.
[0061] Example 9
[0062] Adjust the organic diamine in Step S3 to 58 parts by mass of hexanediamine, and adjust the addition amount of the solvent isopropanol to 3148 parts by mass. Other preparation steps are the same as those in Example 7.
[0063] Example 10
[0064] Adjust the solvent in Step S3 to 3127 parts by mass of ethylene glycol monobutyl ether. Other preparation steps are the same as those in Example 7.
[0065] Example 11
[0066] Adjust the addition amount of octamethylcyclotetrasiloxane in Step S2 to 27660 parts by mass; adjust the addition amount of the second intermediate in Step S3 to 3213 parts by mass, and the addition amount of the solvent isopropanol to 3250 parts by mass. Other preparation steps are the same as those in Example 8.
[0067] Comparative Example 1
[0068] Replace 3-methacryloxypropylmethyldimethoxysilane in Step S2 with (aminoethyl)-γ-aminopropylmethyldimethoxysilane, and keep other preparation steps the same as those in Example 7 to obtain the softener of Comparative Example 1.
[0069] Comparative Example 2
[0070] Replace the long-chain alkene in Step S1 with butene, and keep other preparation steps the same as those in Example 7 to obtain the softener of Comparative Example 2.
[0071] Comparative Example 3
[0072] Purchase the commercially available waterproof co-bath silicone oil RY-5660.
[0073] Emulsify the softeners used in the same bath with the waterproofing agent in the above-mentioned examples and comparative examples, and then finish the fabric according to the following steps:
[0074] Emulsification step: By mass, 100 parts by mass of the softeners used in the same bath with the waterproofing agent in the above-mentioned examples or comparative examples, 5 parts of 1303 emulsifier, 200 parts of deionized water, and 2 parts of glacial acetic acid are emulsified in a homogenizing emulsifier to obtain the emulsifier used in the same bath with the waterproofing agent in this application.
[0075] Finishing step: Dip the cotton shuttle fabric in the working solution. The working solution is 20 g / L of the product emulsion of this application and 30 g / L of the waterproofing agent RH-NB-SF89. The liquor pickup rate is 80%. Pre-dry and bake for 45 - 60 s, the temperature is set at 170 °C, and after a moisture regain of 1 hour, evaluate the fabric performance.
[0076] Perform the following performance tests on the original cotton shuttle fabric, the fabric treated only with the waterproofing agent RH-NB-SF89, and the fabric finished with the waterproofing agent RH-NB-SF89 and the softener product of this application, and record the performance test results in Table 1 below.
[0077] 1. Waterproofness test: Test according to AATCC 22—2010 "Water Repellency: Spray Test". 0 points if the fabric surface is completely wetted, 50 points if the fabric surface is completely wetted, 80 points if the spray points on the fabric surface are wetted, 90 points if there are sporadic wetting points on the fabric surface, and 100 points if the fabric surface is not wetted.
[0078] 2. Contact angle test: Drop a drop of water on the treated fabric, and then test it with a contact angle tester. When the contact angle > 90°, it indicates that the fabric has a water-repellent effect; when the contact angle > 150°, it indicates that the fabric has a super water-repellent effect.
[0079] 3. Softness test: According to GB / T18318 "Textiles - Determination of Fabric Bending Length": Place a long strip-shaped specimen on the platform, press the ruler on the specimen, and the long axis of the specimen is parallel to the length direction of the ruler. Move the ruler and the long axis direction of the specimen on the platform at the same time, so that the part of the specimen extending out of the platform is suspended and bends under its own weight. When the head end of the specimen bending downward touches the inclined plane at 41.5 °C with the horizontal, 1 / 2 of the extended length of the specimen is the bending length. The bending stiffness of the specimen is calculated from the bending length and the mass per unit area.
[0080] Specimen: 6 pieces each of warp and weft knitting with a size of 25 mm * 25 mm. Each specimen is measured 4 times, and the average value is taken.
[0081] Bending stiffness calculation: G = mC 3 10 -2
[0082] Where: G——flexural rigidity per unit width, mN·cm;
[0083] m——mass per unit area of the specimen, g / m 2 ;
[0084] C——average bending length of the specimen, cm
[0085] Table 1 Performance test results
[0086] Analyzing Table 1, by comparing the performance test results of Example 1 and Example 2, it can be seen that the adjustment of the number-average molecular weight and addition amount of the bis-end hydrogen-containing silicone oil has little effect on the performance of the final softener product. By comparing the performance test results of Example 1 and Example 3, it can be seen that increasing the carbon chain length in the long-chain alkene can improve the hydrophobicity of the product, but at the same time it will affect the softness of the treated fabric, and the softness of the fabric decreases. Analyzing the performance test results of Example 1 and Example 4, increasing the length of the organosilicon chain segment of the product can reduce the influence of the waterproofing agent, but too long an organosilicon chain segment is also not conducive to the fabric maintaining softness.
[0087] In Examples 5 to 7, the amounts of 3-methacryloxypropylmethyldimethoxysilane and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane in the preparation steps were adjusted respectively. Increasing the amounts of the above two raw materials can improve the hydrophobicity of the fabric and maintain the effect of the waterproofing agent used in the same bath. However, increasing the amount of 3-methacryloxypropylmethyldimethoxysilane has a negative impact on the softness of the fabric, while increasing the amount of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane is beneficial to improving the softness of the fabric.
[0088] Analyzing the performance test results of Examples 8 to 10, the changes in organic diamine and solvent have little effect on the performance of the final product.
[0089] Analyzing the performance test results of Example 8 and Example 11, increasing the molecular weight of the organosilicon chain segment is beneficial to improving the compounding effect when the softener and the waterproofing agent are used in the same bath and avoiding the failure of the waterproofing agent.
[0090] Analyzing the performance test results of Example 7 and Comparative Examples 1 to 3, compared with the currently commercially available waterproof silicone oil used in the same bath, the softener prepared in this application for use in the same bath with the waterproofing agent can maintain a high waterproof level for the treated fabric and at the same time make the fabric have a certain softness, making it more comfortable to wear.
[0091] The softener used in the same bath as the waterproof agent of the present application is compounded by introducing long-chain alkane segments and 3-methacryloxypropylmethyldimethoxysilane segments, which can improve the compatibility with the waterproof agent, avoid the failure of the waterproof agent, and in addition, can obtain better softness and better comfort.
[0092] The above describes the basic principle, main features and advantages of the present application. Those skilled in the art should understand that the present application is not limited by the above embodiments. What is described in the above embodiments and the specification is only the principle of the present application. Without departing from the spirit and scope of the present application, the present application will have various changes and improvements, and these changes and improvements all fall within the scope of the present application claimed. The scope of protection required by the present application is defined by the appended claims and their equivalents.
Claims
1. A softener used in the same bath as a waterproofing agent, characterized in that, The structural general formula is as follows: where m, x, y, z, and a are integers, and 9 ≤ m ≤ 13; 2 ≤ a ≤ 6; 291 ≤ x ≤ 374; 2 ≤ y ≤ 4; 3 ≤ z ≤ 5.
2. A preparation method of a softener used in the same bath as a waterproofing agent, characterized in that, It includes the following steps: S1: React the hydrogen-containing silicone oil with long-chain carbenes under the action of an inert gas and a catalyst to prepare a first intermediate. S2: React the first intermediate, octamethylcyclotetrasiloxane, 3-methacryloxypropylmethyldimethoxysilane, and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane to prepare a second intermediate. S3: React the second intermediate with an organic diamine to prepare the softener used in the same bath as the waterproofing agent.
3. The preparation method according to claim 2, characterized in that, The structural formula of the first intermediate is as follows: where m and n are integers, and 9 ≤ m ≤ 13; 27 ≤ n ≤ 40.
4. The preparation method according to claim 3, characterized in that, The structural formula of the second intermediate is as follows: Where m, n, x, y, z are integers, and 9 ≤ m ≤ 13; 27 ≤ n ≤ 40; 291 ≤ x ≤ 374; 2 ≤ y ≤ 4; 3 ≤ z ≤ 5.
5. The preparation method according to claim 4, characterized in that, By mass, the specific operation of step S1 is as follows: Put 2000-3000 parts of the hydrogen-containing silicone oil with both ends and 336-448 parts of the long-chain carbene into a reaction vessel. Under an inert gas atmosphere, heat up and add a catalyst, and keep warm for a period of time to obtain the first intermediate.
6. The preparation method according to claim 4, wherein By mass, the specific operation of step S2 is as follows: Put 2336-3448 parts of the first intermediate, 20540-27660 parts of octamethylcyclotetrasiloxane, 464-928 parts of 3-methacryloxypropylmethyldimethoxysilane, and 660-1100 parts of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane into a reaction vessel, add 1.3-1.5 parts of tetramethylammonium hydroxide and heat up. Keep warm for a period of time, then continue to heat up and keep warm for another period of time, and remove low-boiling substances under vacuum to obtain the second intermediate.
7. The preparation method according to claim 4, characterized in that, By mass, the specific operation of step S3 is as follows: Put 2500-3300 parts of the second intermediate, 18-58 parts of the organic diamine, and 2518-3358 parts of a solvent into a reaction vessel, heat up and keep warm for a period of time, and add an initiator to obtain the softener used in the same bath as the waterproofing agent.
8. The preparation method according to claim 4, characterized in that, The number of straight-chain main-chain carbon atoms of the long-chain carbene is greater than or equal to 10.
9. The preparation method according to claim 4, characterized in that, The number-average molecular weight of the hydrogen-containing silicone oil with both ends is 2000-5000.
10. A softener product used in the same bath as a waterproofing agent, characterized in that, It includes the following raw materials by mass: 150-250 parts of water, 2-10 parts of an emulsifier, 1-5 parts of glacial acetic acid, and 90-110 parts of the softener used in the same bath as the waterproofing agent as described in claim 1 or the softener used in the same bath as the waterproofing agent prepared by the preparation method as described in claims 2-9.
Citation Information
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