A multi-block organosilicon fabric finishing agent, its preparation method and application

Abstract

This invention provides a multi-block silicone fabric finishing agent, its preparation method, and its application, comprising the following steps: mixing isocyanate and dihydroxyl-terminated long-chain alkyl silicone oil at a molar ratio of (2-6):1, then adding dibutyltin dilaurate to obtain a reactive prepolymer; adding polyether diol dropwise onto the reactive prepolymer to obtain a reactive intermediate; adding N-methyldiethanolamine dropwise onto the reactive intermediate to obtain the multi-block silicone fabric finishing agent; mixing and emulsifying the multi-block silicone fabric finishing agent with an emulsifier, acetic acid, and water to prepare an aqueous working solution; and then padding and setting to obtain the finished cotton fabric, effectively imparting dynamic wetting properties and a high-grade composite hand feel to the cotton fabric.

Description

Technical Field

[0001] This invention belongs to the field of textile finishing agent technology, specifically relating to a multi-block organosilicon textile finishing agent, its preparation method, and its application. Background Technology

[0002] Organosilicon finishing agents can improve the softness, wrinkle resistance, and water repellency of fabrics during finishing processes. However, monopolymer or disordered copolymer organosilicon may have low binding force with fibers, making it difficult to form a film on the fabric surface. This can lead to problems such as yellowing, poor hand feel, poor wash resistance, and excessive water repellency, all of which affect the fabric's requirements for softness, bulkiness, smoothness, breathability, and durability. Currently, by orderly arranging polysiloxane segments with hydrophilic and / or other functionalized segments, multi-block organosilicon fabric finishing agents have been obtained. These agents can further enhance the hand feel of fabrics while maintaining their mechanical properties, hydrophilicity, wash resistance, and weather resistance, building upon the good softness, temperature resistance, and low surface tension of polysiloxanes.

[0003] However, there are still some problems in the development of multi-block silicone fabric finishing agents in the existing technology. For example, patent CN115787301A discloses a polyurethane-modified silicone softener, its preparation method, and its application. The method involves polymerizing isophorone diisocyanate with N-methyldiethanolamine in a first organic solvent, then adding a blocking agent to block the remaining active isocyanate, resulting in a polyurethane prepolymer. Under an acidic catalyst, the obtained polyurethane prepolymer is polymerized with terminal epoxy silicone oil in a second organic solvent to obtain a polyurethane silicone oil component. The terminal epoxy silicone oil is then reacted with polyetheramine in a second organic solvent to obtain a block silicone oil component. The obtained polyurethane silicone oil component and block silicone oil component are compounded in a predetermined ratio, and then emulsified with an emulsifier to finally obtain the polyurethane-modified silicone softener. This method limits the control of flexible segments by polymerizing polyurethane segments only through isophorone diisocyanate and N-methyldiethanolamine. Furthermore, the separate preparation of the polyurethane silicone oil component and the block silicone oil component before compounding may result in uneven distribution of crosslinking points. Therefore, the development of multi-block silicone fabric finishing agents is of great significance. Under the unified leadership of the head office, the applicant of this invention overcame the relevant technical difficulties. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides a multi-block organosilicon fabric finishing agent, its preparation method, and its applications. The purpose of this invention is to solve the problem of insufficient film looseness and three-dimensionality in fabrics treated by polyether amino silicone oils by preventing the close packing between polysiloxane molecular chains through long-chain alkyl groups. A further objective of this invention is to impart dynamic wetting properties and a composite hand feel of fluffiness, smoothness, and softness to cotton fabrics by constructing linear block copolymers with controllable and specific arrangements of polyurethane segments, organosilicon segments, and polyether segments.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: On the one hand, the present invention provides a multi-block organosilicon fabric finishing agent having the following main chain structure: ; In the main chain structure, the general formula of R1 is as follows: ; The number-average molecular weight of R1 is 2000-8000, and C8-C are grafted onto its side chains. 22 The long-chain alkane group, n and m are the number of repeating units, 2-10.

[0006] Preferably, in the general formula of R1, R' is C8-C 22 Long-chain alkane group -C n H 2n+1 R represents the polyether segment -(CH2CH2O)- n The number average molecular weight is 200-600.

[0007] Preferably, in the main chain structure, R2 is one or more of tolyl, m-phenylenedimethyl, hexamethylene, isophorone, 4,4'-dicyclohexylmethyl, diphenylmethane, and dicyclohexylmethyl; R3 is a polyether segment -(CH2CH2O)- n The number average molecular weight is 400-4000, n is the number of repeating units 2-7; R4 is the chain -CH2CH2N(CH3)CH2CH2-.

[0008] On the other hand, the present invention provides a method for preparing the above-mentioned multi-block organosilicon fabric finishing agent, comprising the following steps: S1: After mixing isocyanate and long-chain alkyl silicone oil with dihydroxyl-terminated alcohols at a molar ratio of (2-6): 1, dibutyltin dilaurate is added to obtain a reactive prepolymer; S2: Add polyether diol dropwise onto the reactive prepolymer to obtain the reaction intermediate; S3: N-methyldiethanolamine is added dropwise to the reaction intermediate to obtain a multi-block organosilicon fabric finishing agent.

[0009] This invention, by introducing long-chain alkyl groups, effectively prevents the close packing of polysiloxane molecular chains, increases the intermolecular distance, and allows for a more porous and three-dimensional film formed on the fiber surface during cotton fabric finishing. Simultaneously, the rigidity and spatial volume of the long-chain alkyl side chains provide physical support between fibers. This invention, by controlling the amounts of isocyanate, dihydroxyl-terminated long-chain alkyl silicone oil, polyether diol, and N-methyldiethanolamine and conducting a stepwise reaction, promotes the formation of an ordered linear block copolymer of polyurethane segments, silicone segments, and polyether segments. The synergistic effect between soft and hard segments enhances the composite feel, effectively improving bulk, smoothness, and softness, forming hydrophilic channels, and imparting dynamic wetting properties to cotton fabrics.

[0010] Preferably, the amount of dibutyltin dilaurate added is 20-40 ppm.

[0011] Preferably, the polyether diol is 30-60% isocyanate by molar percentage; the N-methyldiethanolamine is 30-60% isocyanate.

[0012] Preferably, the reaction conditions for S1 are: under inert gas protection, at 70-75°C, for 2-3 hours.

[0013] Preferably, the reaction conditions for S2 are 75-80°C for 2-3 hours.

[0014] Preferably, the reaction conditions for S3 are 75-80°C for 5-7 hours.

[0015] Preferably, the isocyanate is one or more of isophorone diisocyanate, dicyclohexane 4,4'-diisocyanate, and toluene diisocyanate.

[0016] Preferably, the dual-terminated hydroxyl long-chain alkyl silicone oil has an Mn of 4500-7500 and C8-C8 grafted onto its side chains. 12 Long-chain alkane groups.

[0017] Preferably, the polyether diol is polyethylene glycol with Mn=1000-2000.

[0018] On the other hand, the present invention provides an application of the multi-block organosilicon fabric finishing agent based on the above-mentioned preparation method or the multi-block organosilicon fabric finishing agent obtained by the above-mentioned preparation method in cotton fabric finishing, including the following steps: S1: By weight, 10-20 parts of multi-block silicone fabric finishing agent, 1-5 parts of emulsifier, 1-5 parts of acetic acid, and 50-200 parts of water are mixed and emulsified to prepare an aqueous working solution with a concentration of 10-50 g / L and a pH value of 5-7. S2: The cotton fabric is immersed in the working solution, and after padding, the liquid content of the cotton fabric is 50-100%, thus obtaining the padded cotton fabric. S3: The impregnated cotton fabric is baked in a setting machine at 120-180℃ for 1-5 minutes to obtain the finished cotton fabric.

[0019] Preferably, the static water contact angle of the treated cotton fabric is ≤90° and the water droplet diffusion time is ≤2s.

[0020] Compared with the prior art, the present invention has the following beneficial effects: This invention controls the lengths of soft and hard segments by using isocyanate, dihydroxyl-terminated long-chain alkyl silicone oil, polyether diol, and N-methyldiethanolamine in a stepwise reaction, effectively improving the balance between hand feel and hydrophilicity. This invention controllably arranges polyurethane, silicone, and polyether segments to achieve a synergistic effect between soft and hard segments. The silicone segments effectively accumulate on the fiber surface to provide a soft and smooth feel, the polyether segments interweave to provide hydrophilicity, and the polyurethane segments provide crosslinking points, enriching the fiber surface through hydrogen bonds and molecular chain entanglement. This forms a continuous polymer membrane structure with an elastic network, achieving a balance of softness, smoothness, hydrophilicity, and washability within a polymer system. Attached Figure Description

[0021] Figure 1 The images show comparative test results of the hydrophilicity of cotton fabrics treated with finishing agents (a is Comparative Example 1, b is Example 1). Detailed Implementation

[0022] The present invention will be further described in detail below with reference to specific embodiments. The embodiments given are only for illustrating the present invention and are not intended to limit the scope of the present invention.

[0023] General Implementation Examples A multi-block organosilicon fabric finishing agent has the following main chain structure: ; In the main chain structure, the general formula of R1 is as follows: ; The number-average molecular weight of R1 is 2000-8000, and C8-C are grafted onto its side chains. 22 The long-chain alkane group, n and m are the number of repeating units, 2-10.

[0024] In some embodiments of the present invention, in the general formula of R1, R' is C8-C 22 Long-chain alkane group -C n H 2n+1R represents the polyether segment -(CH2CH2O)- n The number average molecular weight is 200-600.

[0025] In some embodiments of the present invention, in the main chain structure, R2 is one or more of tolyl, m-phenylenedimethyl, hexamethylene, isophorone, 4,4'-dicyclohexylmethyl, diphenylmethane, and dicyclohexylmethyl; R3 is a polyether segment -(CH2CH2O)- n The number average molecular weight is 400-4000, n is the number of repeating units 2-7; R4 is the chain -CH2CH2N(CH3)CH2CH2-.

[0026] A method for preparing a multi-block organosilicon fabric finishing agent based on the above includes the following steps: S1: Under inert gas protection, isocyanate and long-chain alkyl silicone oil with dihydroxyl-terminated alcohols are mixed at a molar ratio of (2-6): 1, and 20-40 ppm of dibutyltin dilaurate is added. The mixture is reacted at 70-75°C for 2-3 hours to obtain the reactive prepolymer. S2: Add 30-60% of polyether diol (molar percentage of isocyanate) to the reaction prepolymer and react at 75-80℃ for 2-3 hours to obtain the reaction intermediate; S3: Add 30-60% N-methyldiethanolamine (molar percentage of isocyanate) to the reaction intermediate and react at 75-80℃ for 5-7 hours to obtain a multi-block organosilicon fabric finishing agent.

[0027] In some embodiments of the present invention, the isocyanate is one or more selected from isophorone diisocyanate, dicyclohexane 4,4'-diisocyanate, and toluene diisocyanate; the bi-terminated alcohol hydroxyl long-chain alkyl silicone oil has Mn=4500-7500 and C8-C8 grafted onto its side chains. 12 The polyether diol is polyethylene glycol, Mn=1000-2000.

[0028] The application of a multi-block silicone fabric finishing agent based on the above-mentioned preparation method in cotton fabric finishing includes the following steps: S1: By weight, 10-20 parts of multi-block silicone fabric finishing agent, 1-5 parts of emulsifier, 1-5 parts of acetic acid, and 50-200 parts of water are mixed and emulsified to prepare an aqueous working solution with a concentration of 10-50 g / L and a pH value of 5-7. S2: The cotton fabric is immersed in the working solution, and after padding, the liquid content of the cotton fabric is 50-100%, thus obtaining the padded cotton fabric. S3: The impregnated cotton fabric is baked in a setting machine at 120-180℃ for 1-5 minutes to obtain the finished cotton fabric.

[0029] In some embodiments of the present invention, the static water contact angle of the treated cotton fabric is ≤90° and the water droplet diffusion time is ≤2s.

[0030] Example 1

[0031] The preparation and application of a multi-block organosilicon fabric finishing agent includes the following steps: S1: Under inert gas protection, isophorone diisocyanate and bi-hydroxyl-terminated long-chain alkyl silicone oil are thoroughly mixed at a molar ratio of 6:1, and then 20 ppm of dibutyltin dilaurate is added. The mixture is reacted at 75°C for 2 hours to obtain a reactive prepolymer. The isocyanate is isophorone diisocyanate. The bi-hydroxyl-terminated long-chain alkyl silicone oil has a Mn of 4500 and C8 long-chain alkane groups grafted onto its side chains. S2: Add 30-60% polyethylene glycol (molar percentage of isophorone diisocyanate) to the reaction prepolymer and react at 80°C for 2 hours to obtain the reaction intermediate; wherein the polyether diol is polyethylene glycol with Mn=1000. S3: 30-60% N-methyldiethanolamine, which is isophorone diisocyanate by molar percentage, is added dropwise to the reaction intermediate and reacted at 75°C for 6 hours to obtain a multi-block organosilicon fabric finishing agent. S4: Weigh out 20 parts by weight of multi-block silicone fabric finishing agent, 3 parts by weight of emulsifier 477, 2 parts by weight of acetic acid and 60 parts by weight of water; mix and emulsify the multi-block silicone fabric finishing agent, emulsifier, acetic acid and water thoroughly to prepare an aqueous working solution with a concentration of 20 g / L and a pH value of 5. S5: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S6: The impregnated cotton fabric is baked in a setting machine at 170°C for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0032] Example 2

[0033] The preparation and application of a multi-block organosilicon fabric finishing agent includes the following steps: S1: Under inert gas protection, dicyclohexane 4,4'-diisocyanate and bi-hydroxyl-terminated long-chain alkyl silicone oil are thoroughly mixed at a molar ratio of 5:1, and then 40 ppm of dibutyltin dilaurate is added. The mixture is reacted at 75°C for 3 hours to obtain a reactive prepolymer. The isocyanate is dicyclohexane 4,4'-diisocyanate; the bi-hydroxyl-terminated long-chain alkyl silicone oil has a Mn of 7500 and C8 long-chain alkane groups grafted onto its side chains. S2: 30-60% polyethylene glycol, which is dicyclohexane 4,4'-diisocyanate by molar percentage, is added dropwise to the reaction prepolymer and reacted at 80°C for 3 hours to obtain the reaction intermediate; wherein, the polyether diol is polyethylene glycol with Mn=2000; S3: 30-60% N-methyldiethanolamine, which is dicyclohexane 4,4'-diisocyanate by molar percentage, is added dropwise to the reaction intermediate and reacted at 75°C for 7 hours to obtain a multi-block organosilicon fabric finishing agent. S4: Weigh out 20 parts by weight of multi-block silicone fabric finishing agent, 6 parts by weight of emulsifier 488, 2 parts by weight of acetic acid and 80 parts by weight of water; mix and emulsify the multi-block silicone fabric finishing agent, emulsifier, acetic acid and water thoroughly to prepare an aqueous working solution with a concentration of 25 g / L and a pH value of 5. S5: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S6: The impregnated cotton fabric is baked in a setting machine at 170°C for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0034] Example 3

[0035] The preparation and application of a multi-block organosilicon fabric finishing agent includes the following steps: S1: Under inert gas protection, isophorone diisocyanate and dihydroxyl-terminated long-chain alkyl silicone oil were thoroughly mixed at a molar ratio of 6:1, and then 20 ppm of dibutyltin dilaurate was added. The mixture was reacted at 75°C for 2 hours to obtain a reactive prepolymer. The isocyanate was isophorone diisocyanate; the dihydroxyl-terminated long-chain alkyl silicone oil had a Mn of 4500 and C2C ... 12 Long-chain alkane groups; S2: Add 30-60% polyethylene glycol (in molar percentage as isophorone diisocyanate) to the reaction prepolymer and react at 80°C for 3 hours to obtain the reaction intermediate; wherein the polyether diol is polyethylene glycol with Mn=1000. S3: 30-60% N-methyldiethanolamine, which is isophorone diisocyanate by molar percentage, is added dropwise to the reaction intermediate and reacted at 75°C for 6 hours to obtain a multi-block organosilicon fabric finishing agent. S4: Weigh out 20 parts by weight of multi-block silicone fabric finishing agent, 3 parts by weight of emulsifier 477, 2 parts by weight of acetic acid and 60 parts by weight of water; mix and emulsify the multi-block silicone fabric finishing agent, emulsifier, acetic acid and water thoroughly to prepare an aqueous working solution with a concentration of 20 g / L and a pH value of 5. S5: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S6: The impregnated cotton fabric is baked in a setting machine at 170°C for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0036] Example 4

[0037] The preparation and application of a multi-block organosilicon fabric finishing agent includes the following steps: S1: Under inert gas protection, toluene diisocyanate and dihydroxyl-terminated long-chain alkyl silicone oil were thoroughly mixed at a molar ratio of 4:1, and then 20 ppm of dibutyltin dilaurate was added. The mixture was reacted at 80°C for 2 hours to obtain a reactive prepolymer. The isocyanate was toluene diisocyanate; the dihydroxyl-terminated long-chain alkyl silicone oil had a Mn of 7500 and C2C ... 12 Long-chain alkane groups; S2: Add 30-60% polyethylene glycol (toluene diisocyanate by molar percentage) to the reaction prepolymer and react at 80°C for 3 hours to obtain the reaction intermediate; wherein the polyether diol is polyethylene glycol with Mn=2000. S3: 30-60% N-methyldiethanolamine (toluene diisocyanate by molar percentage) was added dropwise to the reaction intermediate and reacted at 75°C for 7 hours to obtain a multi-block organosilicon fabric finishing agent. S4: Weigh out 20 parts by weight of multi-block silicone fabric finishing agent, 4 parts by weight of emulsifier 488, 2 parts by weight of acetic acid and 100 parts by weight of water; mix and emulsify the multi-block silicone fabric finishing agent, emulsifier, acetic acid and water thoroughly to prepare an aqueous working solution with a concentration of 25 g / L and a pH value of 5. S5: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S6: The impregnated cotton fabric is baked in a setting machine at 170°C for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0038] Example 5

[0039] The preparation and application of a multi-block organosilicon fabric finishing agent includes the following steps: S1: Under inert gas protection, isophorone diisocyanate and bi-hydroxyl-terminated long-chain alkyl silicone oil are thoroughly mixed at a molar ratio of 2:1, and then 30 ppm of dibutyltin dilaurate is added. The mixture is reacted at 75°C for 2 hours to obtain a reactive prepolymer. The isocyanate is isophorone diisocyanate, and the bi-hydroxyl-terminated long-chain alkyl silicone oil has a Mn of 4500 and C8 long-chain alkane groups grafted onto its side chains. S2: Add 30-60% polyethylene glycol (molar percentage of isophorone diisocyanate) to the reaction prepolymer and react at 80°C for 2 hours to obtain the reaction intermediate; wherein the polyether diol is polyethylene glycol with Mn=1000. S3: 30-60% N-methyldiethanolamine, which is isophorone diisocyanate by molar percentage, is added dropwise to the reaction intermediate and reacted at 75°C for 6 hours to obtain a multi-block organosilicon fabric finishing agent. S4: Weigh out 15 parts of multi-block silicone fabric finishing agent, 2.5 parts of emulsifier 477, 2 parts of acetic acid, and 60 parts of water by weight; mix and emulsify the multi-block silicone fabric finishing agent, emulsifier, acetic acid, and water thoroughly to prepare an aqueous working solution with a concentration of 20 g / L and a pH value of 5. S5: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S6: The impregnated cotton fabric is baked in a setting machine at 170°C for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0040] Example 6

[0041] The preparation and application of a multi-block organosilicon fabric finishing agent includes the following steps: S1: Under inert gas protection, isophorone diisocyanate and bi-hydroxyl-terminated long-chain alkyl silicone oil are thoroughly mixed at a molar ratio of 6:1, and then 20 ppm of dibutyltin dilaurate is added. The mixture is reacted at 75°C for 2 hours to obtain a reactive prepolymer. The isocyanate is isophorone diisocyanate. The bi-hydroxyl-terminated long-chain alkyl silicone oil has a Mn of 4500 and C8 long-chain alkane groups grafted onto its side chains. S2: Add 30-60% polyethylene glycol (molar percentage of isophorone diisocyanate) to the reaction prepolymer and react at 80°C for 2 hours to obtain the reaction intermediate; wherein the polyether diol is polyethylene glycol with Mn=1000. S3: 30-60% N-methyldiethanolamine, which is isophorone diisocyanate by molar percentage, is added dropwise to the reaction intermediate and reacted at 75°C for 6 hours to obtain a multi-block organosilicon fabric finishing agent. S4: Weigh out 10 parts by weight of multi-block silicone fabric finishing agent, 1 part of emulsifier 477, 2 parts of acetic acid, and 50 parts of water; mix and emulsify the multi-block silicone fabric finishing agent, emulsifier, acetic acid, and water thoroughly to prepare an aqueous working solution with a concentration of 30 g / L and a pH value of 5. S5: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S6: The impregnated cotton fabric is baked in a setting machine at 170°C for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0042] Comparative Example 1 An application of an organosilicon fabric finishing agent includes the following steps: S1: Weigh out 20 parts by weight of hydrophilic polyurethane modified silicone oil additive 1035N, 3 parts by weight of emulsifier 477, 2 parts by weight of acetic acid, and 60 parts by weight of water; mix and emulsify the hydrophilic polyurethane modified silicone oil additive 1035N, emulsifier, acetic acid, and water thoroughly to prepare an aqueous working solution with a concentration of 20 g / L and a pH value of 5. S2: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S3: The impregnated cotton fabric is baked in a setting machine at 170℃ for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0043] Comparative Example 2 An application of an organosilicon fabric finishing agent includes the following steps: S1: Weigh out 20 parts of hydrophilic polyurethane modified silicone oil additive 1035N, 6 parts of emulsifier 488, 2 parts of acetic acid, and 80 parts of water by weight; mix and emulsify the hydrophilic polyurethane modified silicone oil additive 1035N, emulsifier, acetic acid, and water thoroughly to prepare an aqueous working solution with a concentration of 25 g / L and a pH value of 5. S2: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S3: The impregnated cotton fabric is baked in a setting machine at 170℃ for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0044] Comparative Example 3 The preparation and application of an organosilicon fabric finishing agent includes the following steps: S1: Under inert gas protection, isophorone diisocyanate and bihydroxyl-terminated long-chain alkyl silicone oil are thoroughly mixed at a molar ratio of 7:1, and then 20 ppm of dibutyltin dilaurate is added. The mixture is reacted at 75°C for 2 hours to obtain a reactive prepolymer. The isocyanate is isophorone diisocyanate. The bihydroxyl-terminated long-chain alkyl silicone oil has a Mn of 4500 and C8 long-chain alkane groups grafted onto its side chains. S2: Add 30-60% polyethylene glycol (molar percentage of isophorone diisocyanate) to the reaction prepolymer and react at 80°C for 2 hours to obtain the reaction intermediate; wherein the polyether diol is polyethylene glycol with Mn=1000. S3: 30-60% N-methyldiethanolamine, which is isophorone diisocyanate by molar percentage, is added dropwise to the reaction intermediate and reacted at 75°C for 6 hours to obtain an organosilicon fabric finishing agent. S4: Weigh out 20 parts of silicone fabric finishing agent, 3 parts of emulsifier 477, 2 parts of acetic acid, and 60 parts of water by weight; mix the silicone fabric finishing agent, emulsifier, acetic acid, and water thoroughly to prepare an aqueous working solution with a concentration of 20 g / L and a pH value of 5. S5: Immerse the cotton fabric in the working solution, and roll it to make the liquid content of the cotton fabric 80%, thus obtaining the impregnated cotton fabric. S6: The impregnated cotton fabric is baked in a setting machine at 170°C for 2 minutes to allow the working solution to form a film on the fiber surface, resulting in the finished cotton fabric. After one day of rehydration, the hand feel and hydrophilicity of the cotton fabric are evaluated.

[0045] Test Example 1 Hydrophilicity tests were conducted on the cotton fabrics obtained in Examples 1-6 and Comparative Examples 1-3. The test results show that the cotton fabrics obtained in Examples 1-6 exhibit excellent hydrophilicity, with a static water contact angle ≤90° and a droplet wetting and diffusion time ≤2s. The hydrophilicity test results for the cotton fabric obtained in Example 1 are shown in the figure below. Figure 1 As shown in (b), the hydrophilicity test diagram of the cotton fabric obtained in Comparative Example 1 is as follows. Figure 1 As shown in (a), compared with Example 1, the cotton fabric obtained in Comparative Example 1 has poor hydrophilicity. Water droplets did not completely wet the fabric after 2 seconds and appeared as water droplets on the cotton fabric.

[0046] Test Example 2 Hand feel tests were conducted on the cotton fabrics obtained in Examples 1-6 and Comparative Examples 1-3. The treated fabrics were graded by touch in groups of 5-10 people, with hand feel divided into 5 levels, including fluffiness, smoothness, and softness. Untreated blank fabric was designated as level 1, with higher levels indicating better hand feel. The test results are shown in Table 1.

[0047] Table 1 As shown in Table 1, the cotton fabric treated with the multi-block silicone fabric finishing agent of the present invention in Example 1 has a bulkiness of level 3, a smoothness of level 4, and a softness of level 4, exhibiting a good high-grade composite hand feel. Verification showed that the bulkiness of the cotton fabrics prepared in Examples 1-6 was superior to that of Comparative Examples 1-3. This is because long-chain alkyl groups can prevent the close packing between polysiloxane molecular chains, increase the intermolecular distance, and promote a more porous and three-dimensional film formed by the finishing agent on the fiber surface. Simultaneously, the long-chain alkyl side chains themselves possess a certain rigidity and spatial volume, which can provide some physical support between the fibers. Furthermore, since the multi-block silicone fabric finishing agent of the present invention is a linear multi-block copolymer with controllable and specific arrangements of polyurethane segments, silicone segments, and polyether segments, its comprehensive characteristics of hydrophilicity, smoothness, and softness are significantly superior to those of Comparative Examples 1-3. Comparative Example 1, treated with a finishing agent, yielded a cotton fabric with a bulkiness grade of 1, a smoothness grade of 3, and a softness grade of 4. Comparative Example 2, also treated with a finishing agent, exhibited a bulkiness grade of 1, a smoothness grade of 3, and a softness grade of 3. Both Comparative Examples 1 and 2 showed poor bulkiness because the organosilicon components used in both examples lacked long-chain alkanes on their side chains. Comparative Example 3, treated with a finishing agent, yielded a cotton fabric with a bulkiness grade of 3, a smoothness grade of 3, and a softness grade of 3. Compared to Example 1, the molar ratio of isophorone diisocyanate to dihydroxyl-terminated long-chain alkyl silicone oil was too high, resulting in a decrease in smoothness and softness.

[0048] Example 1: The hydrophilicity of cotton fabric treated with the multi-block organosilicon fabric finishing agent of the present invention is shown in [reference needed]. Figure 1 (b) The prepared cotton fabric exhibits excellent hydrophilicity, with a static water contact angle ≤90° and a droplet wetting and diffusion time ≤2s. Verification confirmed that the cotton fabrics prepared in Examples 1-6 all possess excellent hydrophilicity, exhibiting a static water contact angle ≤90° and a droplet wetting and diffusion time ≤2s. The hydrophilicity of the cotton fabric obtained by the finishing agent in Comparative Example 1 is shown in [reference needed]. Figure 1 (a) Compared to Example 1, the prepared cotton fabric has poor hydrophilicity. Water droplets did not completely wet the fabric after 2 seconds and appeared as water droplets on the cotton fabric. It was verified that the cotton fabric prepared in Comparative Example 2 had better hydrophilicity, and the time for water droplets to completely wet the fabric was significantly longer than 2 seconds.

Claims

1. A multi-block organosilicon fabric finishing agent, characterized in that, It has the following main chain structure: ； In the main chain structure, the general formula of R1 is as follows: ； The number-average molecular weight of R1 is 2000-8000, and C8-C are grafted onto its side chains. 22 The long-chain alkane group, n and m are the number of repeating units, 2-10.

2. The multi-block organosilicon fabric finishing agent according to claim 1, characterized in that, In the general formula of R1, R' is C8-C 22 Long-chain alkane group -C n H 2n+1 ; R represents the polyether segment -(CH2CH2O)- n The number average molecular weight is 200-600.

3. The multi-block organosilicon fabric finishing agent according to claim 2, characterized in that, In the main chain structure, R2 is one or more of tolyl, m-phenylenedimethyl, hexamethylene, isophorone, 4,4'-dicyclohexylmethyl, diphenylmethane, and dicyclohexylmethyl. R3 represents the polyether segment -(CH2CH2O)- n The number-average molecular weight is 400-4000, and n is the number of repeating units, 2-7. R4 is a chain -CH2CH2N(CH3)CH2CH2-.

4. A method for preparing a multi-block organosilicon fabric finishing agent according to any one of claims 1-3, characterized in that, Includes the following steps: S1: After mixing isocyanate and long-chain alkyl silicone oil with dihydroxyl-terminated alcohols at a molar ratio of (2-6): 1, dibutyltin dilaurate is added to obtain a reactive prepolymer; S2: Add polyether diol dropwise onto the reactive prepolymer to obtain the reaction intermediate; S3: N-methyldiethanolamine is added dropwise to the reaction intermediate to obtain a multi-block organosilicon fabric finishing agent.

5. The method for preparing a novel comb-structured polyether amino silicone oil according to claim 4, characterized in that, The amount of dibutyltin dilaurate added is 20-40 ppm.

6. The method for preparing a multi-block organosilicon fabric finishing agent according to claim 5, characterized in that, The polyether diol is 30-60% isocyanate by molar percentage. The N-methyldiethanolamine is 30-60% isocyanate.

7. The method for preparing a multi-block organosilicon fabric finishing agent according to claim 4, characterized in that, The reaction conditions for S1 are: under inert gas protection, at 70-75°C, for 2-3 hours. The reaction conditions for S2 are 75-80℃ for 2-3 hours; The reaction conditions for S3 are 75-80℃ for 5-7 hours.

8. The method for preparing a multi-block organosilicon fabric finishing agent according to claim 4, characterized in that, The isocyanate is one or more of isophorone diisocyanate, dicyclohexane 4,4'-diisocyanate, and toluene diisocyanate; The bi-terminated hydroxyl-terminated long-chain alkyl silicone oil has an Mn of 4500-7500 and C8-C8 grafted onto its side chains. 12 Long-chain alkane groups; The polyether diol is polyethylene glycol, with Mn=1000-2000.

9. The application of a multi-block organosilicon fabric finishing agent based on any one of claims 1-3 or a multi-block organosilicon fabric finishing agent obtained by the preparation method according to any one of claims 4-8 in cotton fabric finishing, characterized in that, Includes the following steps: S1: By weight, 10-20 parts of multi-block silicone fabric finishing agent, 1-5 parts of emulsifier, 1-5 parts of acetic acid, and 50-200 parts of water are mixed and emulsified to prepare an aqueous working solution with a concentration of 10-50 g / L and a pH value of 5-7. S2: The cotton fabric is immersed in the working solution, and after padding, the liquid content of the cotton fabric is 50-100%, thus obtaining the padded cotton fabric. S3: The impregnated cotton fabric is baked in a setting machine at 120-180℃ for 1-5 minutes to obtain the finished cotton fabric.

10. The application according to claim 9, characterized in that, The static water contact angle of the treated cotton fabric is ≤90° and the water droplet diffusion time is ≤2s.

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