A softener for use in the same bath as a waterproofing agent, its preparation method and its application

By using a softener with a specific structure in the same bath as a waterproofing agent, and utilizing hydrosilylation and polymerization reactions, the performance conflict problem when waterproofing agents and softeners are compounded is solved, achieving highly efficient hydrophobic and soft effects on fabrics, and making it suitable for a variety of fabric materials.

CN120383735BActive Publication Date: 2026-01-30NINGBO RUNHE HIGH TECH MATERIAL CO LTD
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Patent Information

Application Number
CN202510603006.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-05-12
Publication Date
2026-01-30
Estimated Expiration
2045-05-12

AI Technical Summary

Technical Problem

Existing technologies make it difficult to effectively combine waterproofing agents and softeners in the same bath, resulting in a decrease in the waterproofing effect of fabrics or a worse hand feel, and it is also difficult to achieve stable compounding on different fabric materials.

Method used

A softener with a specific structure is used to introduce long-chain alkanes through a hydrosilylation reaction. This is combined with the polymerization reaction of polysiloxane segments and 3-methacryloyloxypropylmethyldimethoxysilane to form directional adsorption, thereby improving the hydrophobicity and softness of the fabric.

Benefits of technology

While maintaining the waterproof effect of the fabric, it significantly improves the hand feel, reduces surface tension, enhances hydrophobic properties, and achieves stable compounding on different fabric materials.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

This application discloses a softener for use in conjunction with a waterproofing agent, its preparation method, and its application. The preparation method includes the following steps: S1: reacting a double-ended hydrogen-containing silicone oil with a long-chain carbide under the action of an inert gas and a catalyst to prepare a first intermediate; S2: reacting the first intermediate, octamethylcyclotetrasiloxane, 3-methacryloyloxypropylmethyldimethoxysilane, and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane to prepare a second intermediate; S3: reacting the second intermediate with an organic diamine to prepare the softener for use in conjunction with the waterproofing agent. The softener of this application, used in conjunction with a waterproofing agent, can maintain good waterproofing while improving fabric softness.
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Description

Technical Field

[0001] This application relates to the field of polymer materials, specifically to a softener used in the same bath as a waterproofing agent, its preparation method, and its application. Background Technology

[0002] With the continued growth in market demand for functional textiles such as outdoor sportswear, medical protective clothing, and home textiles, the demand for composite functional fabrics that combine waterproofing, softness, and durability has risen sharply. Traditional single-function finishing technologies can no longer meet the needs of high-end consumer and industrial applications. In traditional textile finishing processes, waterproofing and softening functions must be achieved in two steps using a two-bath method, i.e., waterproofing treatment is performed first, followed by softening treatment. This process has problems such as complex procedures, long processing cycles, large wastewater discharge, and high production costs. In addition, the ionic conflict between waterproofing agents and softeners, such as when cationic waterproofing agents are mixed with anionic softeners, can easily lead to a decline in product performance, making it difficult to simultaneously achieve both waterproofing and softness.

[0003] In recent years, continuous innovation in auxiliary agent formulation technology, the application of C6 waterproofing agents, and the optimization of compatibility between nonionic / cationic softeners, combined with the application of nanotechnology, have made it possible to achieve waterproofing and softening functions synergistically in a single bath. By rationally compounding softeners and waterproofing agents, the one-bath process can significantly reduce water consumption, energy consumption, and chemical usage, promoting the textile industry's transformation towards green and low-energy consumption, aligning with the concept of sustainable development.

[0004] Currently, products that can be effectively compounded with waterproofing agents, have minimal impact on waterproofing performance, and improve the hand feel of fabrics after waterproofing treatment are relatively scarce in the market. Most softeners, when mixed with waterproofing agents, significantly weaken the hydrophobic effect due to differences in chemical structure and ionic conflicts, resulting in fabrics failing to meet expected waterproofing standards. Even some products that can guarantee waterproofing performance struggle to effectively address the stiffness and roughness of fabrics after waterproofing treatment, severely impacting wearing comfort and product added value. Furthermore, products that meet the requirements of large-scale industrial production and achieve stable compounding effects across different fabric materials (such as cotton, polyester, and nylon) are extremely rare due to current technological limitations. Therefore, products that can overcome these technological barriers, effectively compound with waterproofing agents, have minimal impact on waterproofing performance, and significantly improve the hand feel of fabrics after waterproofing treatment are in high demand and short supply in the market, urgently requiring innovative technologies to fill this gap. Summary of the Invention

[0005] The purpose of this application is to provide a fabric softener that can be used in the same bath as a waterproofing agent, which can maintain a good waterproofing effect while improving the softness of the fabric.

[0006] To achieve the above objectives, 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, the general structural formula of which is:

[0007] 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.

[0008] This application also provides a method for preparing a softener for use in the same bath as a waterproofing agent, comprising the following steps: S1: reacting a bipolar hydrogen-containing silicone oil with a long-chain carbene under the action of an inert gas and a catalyst to prepare a first intermediate; S2: reacting the first intermediate, octamethylcyclotetrasiloxane, 3-methacryloyloxypropylmethyldimethoxysilane, and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane to prepare a second intermediate; S3: reacting the second intermediate with an organic diamine to prepare the softener for use in the same bath as the waterproofing agent.

[0009] As a preferred embodiment, the structural formula of the first intermediate is:

[0010] Where m and n are integers, and 9≤m≤13; 27≤n≤40.

[0011] As another preferred option, the structural formula of the second intermediate is:

[0012] Where m, n, x, y, z are integers, and 9≤m≤13; 27≤n≤40; 291≤x≤374; 2≤y≤4; 3≤z≤5.

[0013] As another preferred embodiment, step S1, by mass, specifically involves placing 2000-3000 parts of the bipolar hydrogen-containing silicone oil and 336-448 parts of the long-chain carbene in a reaction vessel, heating and adding a catalyst under an inert gas atmosphere, and maintaining the temperature for a period of time to obtain the first intermediate.

[0014] As another preferred embodiment, step S2, by mass, specifically comprises: placing 2336–3448 parts of the first intermediate, 20540–27660 parts of octamethylcyclotetrasiloxane, 464–928 parts of 3-methacryloyloxypropylmethyldimethoxysilane, and 660–1100 parts of 3-2,3-epoxypropoxypropylmethyldimethoxysilane into a reaction vessel, adding 1.3–1.5 parts of tetramethylammonium hydroxide and heating, maintaining the temperature for a period of time, continuing to heat, maintaining the temperature again for a period of time, and removing low-boiling substances under vacuum to obtain the second intermediate.

[0015] As another preferred embodiment, step S3, by weight, specifically involves placing 2500–3300 parts of the second intermediate, 18–58 parts of the organic diamine, and 2518–3358 parts of the solvent in a reaction vessel, heating and maintaining the temperature for a period of time, and adding an initiator to obtain the softener used in the same bath as the waterproofing agent.

[0016] As another preferred embodiment, the long-chain carbene has a linear main chain with 10 or more carbon atoms.

[0017] Further preferably, the number-average molecular weight of the dual-end hydrogen-containing silicone oil is 2000-5000.

[0018] This application also provides a softener product for use in the same bath as a waterproofing agent, comprising the following raw materials in parts by weight: 150-250 parts water, 2-10 parts emulsifier, 1-5 parts glacial acetic acid, and 90-110 parts softener for use in the same bath as described in claim 1 or softener for use in the same bath as described in claims 2-9.

[0019] Compared with the prior art, the beneficial effects of this application are as follows:

[0020] (1) The softener used in this application with the waterproofing agent has long-chain alkane in its structure. It works together with the polysiloxane chain segments in the structure to reduce the surface tension of the product and improve the hydrophobic properties of the fabric surface after treatment.

[0021] (2) The softener used in the same bath as the waterproofing agent in this application introduces 3-methacryloyloxypropylmethyldimethoxysilane structural segments. 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 methacrylic group can undergo a certain polymerization reaction after high-temperature setting, and together with the polysiloxane, it imparts film-forming properties to the treated fabric, thereby reducing the impact of the waterproofing agent on the softener.

[0022] (3) The softener used in this application in the same bath as the waterproofing agent forms a directional adsorption of polysiloxane and amino groups on the fabric surface when the fabric is treated, which can give the fabric an excellent hand feel and reduce the weakening effect of the softener and waterproofing agent on the hand feel when they are bathed together. Detailed Implementation

[0023] The present application will be further described below with reference to specific embodiments. It should be noted that, without conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments.

[0024] The terms “comprising” and “having”, and any variations thereof, in the specification and claims of this application are intended to cover non-exclusive inclusion, for example, a process, method, system, product, or device that includes a series of steps or units is not necessarily limited to those steps or units that are explicitly listed, but may include other steps or units that are not explicitly listed or that are inherent to such process, method, product, or device.

[0025] This application provides a softener for use in the same bath as a waterproofing agent, with the following general structural formula:

[0026] 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.

[0027] The softener used in this application in the same bath as the waterproofing agent incorporates long-chain alkane into its structure. This alkane, together with the polysiloxane segments in the structure, reduces the surface tension of the product and improves the hydrophobic properties of the fabric surface after treatment.

[0028] The softener used in this application, when bathed with a waterproofing agent, incorporates a 3-methacryloyloxypropylmethyldimethoxysilane structural segment. The ester group enhances the compatibility of the softener with the waterproofing agent. Simultaneously, in the presence of an initiator, the methacrylic group undergoes a polymerization reaction after high-temperature setting, contributing to the film-forming properties of the treated fabric along with the polysiloxane, thereby reducing the impact of the waterproofing agent on the softener.

[0029] The softener used in this application, when bathed with a waterproofing agent, forms a directional adsorption of polysiloxanes and amino groups on the fabric surface during fabric treatment, which can give the fabric an excellent hand feel and reduce the weakening effect of the softener on the hand feel when bathed with a waterproofing agent.

[0030] This application also provides a method for preparing a softener for use in the same bath as a waterproofing agent, comprising the following steps:

[0031] S1: The first intermediate is prepared by reacting double-ended hydrogen-containing silicone oil with long-chain carbides under the action of an inert gas and a catalyst;

[0032] S2: The first intermediate, octamethylcyclotetrasiloxane, 3-methacryloyloxypropylmethyldimethoxysilane and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane are reacted to prepare the second intermediate;

[0033] S3: The second intermediate and the organic diamine are reacted to prepare the softener of this application for use in the same bath as the waterproofing agent.

[0034] The structural formula of the first intermediate is as follows: Where m and n are integers, and 9≤m≤13; 27≤n≤40.

[0035] The structural formula of the second intermediate is:

[0036] Where 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, step S1, by mass, specifically involves placing 2000-3000 parts of bipolar hydrogen-containing silicone oil and 336-448 parts of long-chain carbides in a reaction vessel, heating and adding a catalyst under an inert gas atmosphere, and maintaining the temperature for a period of time to obtain the first intermediate.

[0038] The reaction formula for the bipolar hydrogen-containing silicone oil and long-chain carbene in step S1 is as follows:

[0039] Where m and n are integers, and 9≤m≤13; 27≤n≤40.

[0040] In a preferred embodiment, the number of carbon atoms in the straight-chain backbone of the long-chain carbene is greater than or equal to 10.

[0041] In some embodiments, step S2, by mass, specifically comprises: placing 2336–3448 parts of the first intermediate, 20540–27660 parts of octamethylcyclotetrasiloxane, 464–928 parts of 3-methacryloyloxypropylmethyldimethoxysilane, and 660–1100 parts of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane into a reaction vessel, adding 1.3–1.5 parts of tetramethylammonium hydroxide and heating, maintaining the temperature for a period of time, continuing to heat, maintaining the temperature again for a period of time, removing low-boiling substances under vacuum to obtain the second intermediate.

[0042] In step S2, the reaction formulas for the first intermediate, octamethylcyclotetrasiloxane, 3-methacryloyloxypropylmethyldimethoxysilane, and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane are as follows:

[0043] Where m, n, x, y, z are integers, and 9≤m≤13; 27≤n≤40; 291≤x≤374; 2≤y≤4; 3≤z≤5.

[0044] In some embodiments, step S3, by weight, specifically involves placing 2500-3300 parts of the second intermediate, 18-58 parts of the organic diamine, and 2518-3358 parts of the solvent in a reaction vessel, heating and maintaining the temperature for a period of time, adding an initiator, and obtaining the softener of this application for use in the same bath as the waterproofing agent.

[0045] In step S3, the reaction formula for the second intermediate and the organic diamine is as follows:

[0046] 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.

[0047] This technology utilizes a hydrosilylation reaction to introduce long-chain alkane structures as end-capping agents. The introduction of long-chain alkanes effectively reduces surface tension, thereby improving the hydrophobic properties of the product. By utilizing the cleavage and rearrangement of siloxane segments, 3-methacryloyloxypropylmethyldimethoxysilane is introduced into the product structure. The methacrylic structure, under high-temperature setting and the action of an initiator, undergoes a certain polymerization reaction, improving the film-forming properties of the product on the fabric surface and thus reducing the impact on the waterproofing effect of the waterproofing agent. Furthermore, by utilizing the reaction between epoxy groups and amino groups, amino groups are introduced into the product structure. The combined effect of polysiloxane segments and amino groups gives the product an excellent soft hand feel.

[0048] This application also provides a softener product for use with a waterproofing agent in the same bath as described in this application, comprising: the softener for use with a waterproofing agent in the same bath as described in this application, emulsifier 1303, water, and glacial acetic acid.

[0049] Example 1

[0050] Prepare a softener for use in the same bath as the waterproofing agent, by weight:

[0051] S1: 2000 parts of bipolar hydrogen-containing silicone oil with a number average molecular weight of 2000 and 336 parts of 1-dodecene were added to a reaction vessel equipped with a thermometer, stirrer and reflux condenser. Nitrogen gas was introduced, the temperature was raised to 75°C, 0.6 parts of caster catalyst were added, the temperature was raised to 110°C and held for 6 hours to obtain the first intermediate.

[0052] S2: 2336 parts of the first intermediate, 21550 parts of octamethylcyclotetrasiloxane, 464 parts of 3-methacryloyloxypropylmethyldimethoxysilane and 660 parts of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane were added to a reaction vessel equipped with a thermometer, stirrer and reflux condenser. The mixture was stirred thoroughly, and 1.3 parts of tetramethylammonium hydroxide were added. The temperature was raised to 100°C and held for 10 hours. The temperature was raised to 135°C and held for 1 hour. The low-boiling substances were removed under a vacuum of -0.09 MPa to obtain the second intermediate.

[0053] S3: Add 2500 parts of the second intermediate, 18 parts of ethylenediamine and 2518 parts of isopropanol to a reaction vessel equipped with a thermometer, stirrer and reflux condenser, stir thoroughly, heat to 78°C, keep warm for 6 hours, add 0.2 parts of azobisisobutyronitrile ethanol solution to prepare a softener for use in the same bath as a waterproofing agent as in Example 1 of this application.

[0054] Example 2

[0055] The number-average molecular weight of the double-ended hydrogen-containing silicone oil in step S1 was adjusted to 3000, and the amount added was adjusted accordingly to 3000 parts by mass. The amount of cassiterite catalyst was adjusted to 0.8 parts by mass.

[0056] The amount of the first intermediate added in step S2 was adjusted to 3336 parts by mass, and the amount of octamethylcyclotetrasiloxane added was adjusted to 20540 parts by mass. Other preparation steps were consistent with the preparation steps in Example 1.

[0057] Example 3

[0058] In step S1, the long-chain carbene was replaced with 1-hexadecene, and the amount added was adjusted to 448 parts by mass. After adding the cassette catalyst, the temperature was raised to 120°C. In step S2, the amount of the first intermediate added was adjusted to 2448 parts by mass, and the amount of octamethylcyclotetrasiloxane added was adjusted to 21430 parts by mass. Other preparation steps were consistent with those in Example 1.

[0059] Example 4

[0060] The amount of octamethylcyclotetrasiloxane added in step S2 was adjusted to 26,430 parts by mass; the amount of the second intermediate added in step S3 was adjusted to 3,000 parts by mass, and the amount of isopropanol solvent added was adjusted to 3,018 parts by mass. Other preparation steps were consistent with those in Example 3.

[0061] Example 5

[0062] The amount of 3-methacryloyloxypropylmethyldimethoxysilane added in step S2 was adjusted to 928 parts by mass; the amount of the second intermediate added in step S3 was adjusted to 3046 parts by mass, and the amount of isopropanol solvent added was adjusted to 3064 parts by mass. Other preparation steps were consistent with the preparation steps in Example 4.

[0063] Example 6

[0064] In step S2, the amount of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane added was adjusted to 1100 parts by mass; in step S3, the amount of the second intermediate added was adjusted to 3044 parts by mass, the amount of ethylenediamine added was adjusted to 30 parts by mass, and the amount of isopropanol solvent added was adjusted to 3074 parts by mass. Other preparation steps were consistent with those in Example 4.

[0065] Example 7

[0066] In step S2, the amount of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane added was adjusted to 1100 parts by mass; in step S3, the amount of the second intermediate added was adjusted to 3090 parts by mass, the amount of ethylenediamine added was adjusted to 30 parts by mass, and the amount of isopropanol solvent added was adjusted to 3120 parts by mass. Other preparation steps remained consistent with those in Example 5.

[0067] Example 8

[0068] In step S3, the organic diamine was adjusted to 37 parts by mass of propylene diamine, and the amount of isopropanol solvent added was adjusted to 3127 parts by mass. The other preparation steps remained consistent with those in Example 7.

[0069] Example 9

[0070] In step S3, the organic diamine was adjusted to 58 parts by mass of hexamethylenediamine, and the amount of isopropanol solvent added was adjusted to 3148 parts by mass. The other preparation steps remained consistent with those in Example 7.

[0071] Example 10

[0072] The solvent in step S3 was adjusted to 3127 parts by mass of ethylene glycol monobutyl ether. The other preparation steps remained consistent with those in Example 7.

[0073] Example 11

[0074] The amount of octamethylcyclotetrasiloxane added in step S2 was adjusted to 27,660 parts by mass; the amount of the second intermediate added in step S3 was adjusted to 3,213 parts by mass, and the amount of isopropanol solvent added was adjusted to 3,250 parts by mass. Other preparation steps were consistent with those in Example 8.

[0075] Comparative Example 1

[0076] In step S2, 3-methacryloyloxypropylmethyldimethoxysilane was replaced with (aminoethyl)-γ-aminopropylmethyldimethoxysilane, while the other preparation steps remained the same as those in Example 7, to obtain Comparative Example 1 softener.

[0077] Comparative Example 2

[0078] The long-chain carbene in step S1 was replaced with butene, and the other preparation steps were kept the same as those in Example 7 to obtain Comparative Example 2 softener.

[0079] Comparative Example 3

[0080] Purchased commercially available waterproof silicone oil RY-5660 for use in the same bath.

[0081] The softeners used in the above embodiments and comparative examples for use in the same bath as the waterproofing agent were emulsified, and then the fabrics were finished according to the following steps:

[0082] Emulsification step: By weight, 100 parts by weight of the softener used in the same bath as the waterproofing agent in each of the above embodiments or comparative examples, 5 parts by weight of 1303 emulsifier, 200 parts by weight of deionized water and 2 parts by weight of glacial acetic acid are emulsified in a homogenizing emulsifier to obtain the emulsifier used in the same bath as the waterproofing agent in this application.

[0083] Finishing steps: The cotton woven fabric is impregnated with the working solution, which is 20g / L of the emulsion of this application and 30g / L of waterproofing agent RH-NB-SF89. The impregnation rate is 80%. The fabric is pre-dried for 45-60 seconds at a temperature of 170℃. After 1 hour of rehydration, the fabric performance is evaluated.

[0084] The following performance tests were conducted on the original cotton woven fabric, the fabric treated only with waterproofing agent RH-NB-SF89, and the fabric treated with both waterproofing agent RH-NB-SF89 and the softener product of this application, and the performance test results are recorded in Table 1 below.

[0085] 1. Water resistance test: According to AATCC 22-2010 "Water repellency: Spray test", the fabric surface is completely wetted, which is 0 points; the fabric surface is completely wetted, which is 50 points; the fabric surface is wetted by spraying, which is 80 points; the fabric surface has a few wetted spots, which is 90 points; and the fabric surface is not wetted, which is 100 points.

[0086] 2. Contact Angle Test: Place a drop of water on the treated fabric and then test it with a contact angle tester. When the contact angle is >90°, it indicates that the fabric has a water-repellent effect; when the contact angle is >150°, it indicates that the fabric has a super water-repellent effect.

[0087] 3. Softness Test: According to GB / T18318 "Textiles - Determination of Bending Length of Fabrics": Place a long strip sample on a platform, with a ruler pressing on the sample, the major axis of the sample parallel to the length direction of the ruler. Move the ruler and the major axis of the sample simultaneously on the platform, causing the portion of the sample extending beyond the platform to be suspended in the air and bend under its own weight. When the downward-bending end of the sample touches an inclined plane at a 41.5° angle to the horizontal, half of the extended length of the sample is the bending length. The bending stiffness of the sample is calculated by the bending length and the mass per unit area.

[0088] Samples: 6 pieces each of 25mm*25mm warp and weft knitted fabrics, each sample was measured 4 times and the average value was taken;

[0089] Bending stiffness calculation: G = mC 3 10 -2

[0090] Where: G—bending stiffness per unit width, mN·cm;

[0091] m — Mass per unit area of ​​the sample, g / m 2 ;

[0092] C—average bending length of the specimen, cm

[0093] Table 1 Performance Test Results

[0094]

[0095]

[0096] Analysis of Table 1, comparing the performance test results of Examples 1 and 2, shows that adjusting the number-average molecular weight and addition amount of the dual-end hydrogen-containing silicone oil has little impact on the performance of the final softener product. A comparison of the performance test results of Examples 1 and 3 shows that increasing the carbon chain length in the long-chain carbides can improve the hydrophobicity of the product, but it will simultaneously affect the softness of the treated fabric, resulting in a decrease in fabric softness. Analysis of the performance test results of Examples 1 and 4 shows that increasing the length of the silicone chain segments in the product can reduce the impact of the waterproofing agent, but excessively long silicone chain segments are also detrimental to maintaining fabric softness.

[0097] Examples 5 through 7 respectively adjusted the amounts of 3-methacryloxypropylmethyldimethoxysilane and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane in the preparation steps. Increasing the amount of the 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.

[0098] Analysis of the performance test results of Examples 8 to 10 shows that changes in the organic diamine and solvent have little impact on the performance of the final product.

[0099] Analysis of the performance test results of Examples 8 and 11 shows that increasing the molecular weight of the organosilicon segments is beneficial to improving the compounding effect when the softener and waterproofing agent are used in the same bath, and avoiding the failure of the waterproofing agent.

[0100] Analyzing the performance test results of Example 7 and Comparative Examples 1 to 3, and comparing them with currently commercially available waterproof silicone oils, the softener used in the waterproofing agent prepared in this application can maintain a high waterproof rating while making the fabric soft and more comfortable to wear after treatment.

[0101] The waterproofing agent and softener used in this application incorporate long-chain alkane segments and 3-methacryloyloxypropylmethyldimethoxysilane segments, which can improve compatibility with the waterproofing agent, prevent the waterproofing agent from failing, and also achieve better softness and comfort.

[0102] The basic principles, main features, and advantages of this application have been described above. Those skilled in the art should understand that this application is not limited to the above embodiments. The embodiments and descriptions in the specification are merely the principles of this application. Various changes and modifications can be made to this application without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claims. The scope of protection claimed by this application is defined by the appended claims and their equivalents.

Claims

1. A softening agent for use in a single bath with a water repellent agent, characterized in that, The structural general formula is: wherein m, x, y, z, a are integers, and 9 < m < 13; 2 < a < 6; 291 < x < 374; 2 < y < 4; 3 < z < 5.

2. A process for the preparation of a softening agent for use in a single bath with a repellent agent as claimed in claim 1, characterized in that, The method comprises the following steps: S1: reacting the double-end hydrogen-containing silicone oil and the long-chain carbene under the action of inert gas and a catalyst to prepare a first intermediate; S2: reacting the first intermediate, octamethylcyclotetrasiloxane, 3-methacryloyloxypropylmethyldimethoxysilane and 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane to prepare a second intermediate; S3: reacting the second intermediate and an organic diamine to prepare the softener for use in the same bath as the waterproof agent.

3. The production method according to claim 2, wherein The structural formula of the first intermediate is: wherein m, n are integers and 9 < m < 13; 27 < n < 40.

4. The production method according to claim 3, wherein The structural formula of the second intermediate 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.

5. The production method according to claim 4, wherein In terms of mass parts, the S1 step specifically comprises: placing 2000-3000 parts of the double-end hydrogen-containing silicone oil and 336-448 parts of the long-chain carbene in a reaction container, heating and adding a catalyst under an inert gas atmosphere, and obtaining the first intermediate after a certain period of incubation.

6. The production method according to claim 4, wherein In terms of mass parts, the S2 step specifically comprises: placing 2336-3448 parts of the first intermediate, 20540-27660 parts of octamethylcyclotetrasiloxane, 464-928 parts of 3-methacryloyloxypropylmethyldimethoxysilane and 660-1100 parts of 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane in a reaction container, adding 1.3-1.5 parts of tetramethylammonium hydroxide and heating, continuing to heat after a certain period of incubation, again incubating for a certain period of time, and removing low-boiling substances under vacuum to obtain the second intermediate.

7. The production method according to claim 4, wherein In terms of mass parts, the S3 step specifically comprises: placing 2500-3300 parts of the second intermediate, 18-58 parts of an organic diamine and 2518-3358 parts of a solvent in a reaction container, heating and incubating for a certain period of time, adding an initiator to obtain the softener for use in the same bath as the waterproof agent.

8. The production method according to claim 4, wherein The number of carbon atoms in the linear main chain of the long-chain carbene is greater than or equal to 10.

9. The production method according to claim 4, wherein The number-average molecular weight of the double-end hydrogen-containing silicone oil is 2000-5000.

10. A softener product for use in a single bath with a water repellent agent, characterized in that, The method comprises the following steps: adding 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 for use in the same bath as the waterproof agent according to claim 1 or the softener for use in the same bath as the waterproof agent prepared by the method according to any one of claims 2-9.

Citation Information

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