Water-washing resistant low-moisture silk quilt and preparation method thereof

Abstract

The present application relates to the technical field of silk quilt, in particular to a water-washing-resistant low-moisture silk quilt and a preparation method thereof.The present application comprises the following steps: S1: adding a hydrophobic finishing agent, a cardanol-enclosed polyisocyanate into water, and then adding branched-chain amino silicone oil, an emulsifier and rosemary acid, and stirring uniformly to obtain a finishing liquid; S2: immersing silk floss pieces into the finishing liquid, taking out, and then washing with water, drying, baking to obtain water-washing-resistant silk floss pieces; opening the water-washing-resistant silk floss pieces, layer-by-layer laying, twisting, fixing to obtain a silk cotton batten, and finally, quilting and sewing positioning to obtain the water-washing-resistant low-moisture silk quilt.

Description

Technical Field

[0001] This invention relates to the field of silk quilt technology, specifically to a washable, low-moisture-regain silk quilt and its preparation method. Background Technology

[0002] In modern family life, silk quilts are widely favored by consumers due to their advantages such as lightness, breathability, and warmth. The main component of silk quilts is natural silk, which is characterized by its excellent moisture absorption and wicking properties, providing users with a comfortable sleeping environment. However, traditional silk quilts often face some problems in practical use.

[0003] As people's demands for quality of life increase, washability and low moisture regain are gradually becoming important factors affecting the competitiveness of silk quilts in the market. Silk quilts are typically difficult to dry after washing, and due to their high moisture absorption, improper storage or use can easily lead to insect infestation, mold, and other problems in humid environments. This undoubtedly affects their lifespan and user experience.

[0004] However, traditional silk quilts are prone to damage to the silk fibers during washing, affecting their warmth and comfort. Furthermore, washed silk quilts often require a long drying time, causing inconvenience. Due to the natural properties of silk, it easily absorbs moisture and tends to become damp in high humidity environments. This not only affects the drying effect of the bedding but may also lead to bacterial growth, thus impacting the user's health.

[0005] Therefore, we propose a water-resistant, low-moisture-regain silk quilt and its preparation method. Summary of the Invention

[0006] The purpose of this invention is to provide a washable, low-moisture silk quilt and its preparation method, so as to solve the problems raised in the prior art.

[0007] To achieve the above objectives, the present invention provides the following technical solution: A method for preparing a washable, low-moisture-regain silk quilt includes the following steps: Step S1: Add the hydrophobic finishing agent and cashew phenol blocked polyisocyanate to water, then add branched amino silicone oil, emulsifier and rosmarinic acid, stir evenly to obtain the finishing solution; Step S2: Immerse the silk floss sheet in the finishing solution, take it out, wash it, dry it, and bake it to obtain a washable silk floss sheet; stretch the washable silk floss sheet, lay it layer by layer, twist it, and fix it to obtain a silk quilt; finally, perform quilting and positioning to obtain a washable, low-moisture silk quilt.

[0008] Furthermore, the finishing solution is composed of 30-50 g / L hydrophobic finishing agent, 10-30 g / L cashew phenol blocked polyisocyanate, 3-5 g / L branched amino silicone oil, 1.5-3.0 g / L emulsifier, and 1-2 g / L rosmarinic acid.

[0009] Furthermore, the preparation method of the hydrophobic finishing agent is as follows: Octadecylamine and deionized water were stirred evenly at 60-70℃ to obtain an aqueous solution of octadecylamine; the aqueous solution of octadecylamine and an aqueous dispersion of tetraethyl orthosilicate were stirred at room temperature for 10-12 h, hexadecyltrimethoxysilane and methyltrimethoxysilane were added, and the mixture was stirred for 1-2 h; finally, γ-aminopropyltriethoxysilane was added, and the mixture was stirred for 3-4 h to obtain a hydrophobic finishing agent.

[0010] Furthermore, the mass ratio of octadecylamine to deionized water is 1:(100-110), and the concentration of the tetraethyl orthosilicate aqueous dispersion is 30-40 wt%.

[0011] Furthermore, the mass ratio of the octadecylamine aqueous solution to the tetraethyl orthosilicate aqueous dispersion is 1:(1-2).

[0012] Furthermore, the mass ratio of the aqueous solution of hexadecyltrimethoxysilane, methyltrimethoxysilane, γ-aminopropyltriethoxysilane and octadecylamine is (1-1.5):2:1:50.

[0013] Furthermore, the preparation method of the cashew phenol blocked polyisocyanate is as follows: Cashew nut phenol, polyisocyanate and ethyl acetate are mixed evenly and reacted at 60-90℃ for 7-10 hours until -NCO is no longer detectable. The solvent is then recovered by vacuum distillation to obtain cashew nut phenol blocked polyisocyanate.

[0014] Furthermore, the molar ratio of the phenolic hydroxyl group of the cashew phenol to the -NCO of the polyisocyanate is (1.1-1.3):1.

[0015] Further, the polyisocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, and HDI-trimer.

[0016] Furthermore, the preparation method of the branched amino silicone oil is as follows: Step A: Mix vinyl dimethylsilanol and N,N-dimethylformamide evenly, replace with nitrogen, add 1,8-diazabicycloundec-7-ene, toluene and hexamethylcyclotrisiloxane, react at room temperature for 4-6 h, add acetic acid to neutralize for 8-10 min, wash with deionized water, remove water from the organic phase with anhydrous sodium sulfate, remove toluene and N,N-dimethylformamide under reduced pressure to obtain α-vinyl-ω-hydroxy polydimethylsiloxane; Step B: Mix α-vinyl-ω-hydroxy polydimethylsiloxane, aminoethylaminopropyltrimethoxysilane and 1,8-diazabicycloundec-7-ene evenly, under nitrogen protection, and react at 70-80℃ for 3-5h. Remove residual reactants at -0.095MPa and 150℃ to obtain the intermediate. Step C: Mix hydroxyl-terminated polydimethylsiloxane and intermediate evenly, under nitrogen protection, heat to 75-85℃, add a mixed solution of potassium hydroxide and water, and react at -0.095MPa for 3-4 hours to obtain branched amino silicone oil.

[0017] Further, in step A, the mass ratio of vinyldimethylsilanol, N,N-dimethylformamide, 1,8-diazabicycloundec-7-ene, toluene and hexamethylcyclotrisiloxane is 1:(0.5-1.0):(0.2-0.4):(2-4):(8-10).

[0018] Further, in step B, the mass ratio of α-vinyl-ω-hydroxy polydimethylsiloxane, aminoethylaminopropyltrimethoxysilane and 1,8-diazabicycloundec-7-ene is 1:(0.6-0.8):(0.02-0.03).

[0019] Further, in step C, the mass ratio of the hydroxyl-terminated polydimethylsiloxane, the intermediate, potassium hydroxide, and water is 100:(9-12):(0.003-0.005):(0.05-0.08).

[0020] Furthermore, the immersion is carried out under vibration at a temperature of 30-50°C for 1-3 hours; the bath ratio (mass) is 1:(10-20).

[0021] Furthermore, the drying temperature is 100-110℃ and the time is 1-2 minutes; the baking temperature is 150-160℃ and the time is 50-70 seconds.

[0022] Compared with the prior art, the beneficial effects of the present invention are: The present invention discloses a water-resistant, low-moisture-regain silk quilt and its preparation method. By compounding a hydrophobic finishing agent, cashew phenol blocked polyisocyanate, branched amino silicone oil, emulsifier, and rosmarinic acid, a finishing solution is obtained, thereby simultaneously achieving the excellent water-resistant performance and long-lasting low-moisture-regain characteristics of the silk quilt.

[0023] In this scheme, the octadecaneamine-siloxane composite nanoparticle dispersion obtained by controlling the hydrolysis of ethyl silicate with an alkaline aqueous solution can successfully disperse long-chain alkyl groups in water. After adding hexadecyltrimethoxysilane, methyltrimethoxysilane and γ-aminopropyltriethoxysilane, a water-based, fluorine-free hydrophobic finishing agent is prepared. This eliminates the need for traditional fluorine-containing finishing agents, avoids persistent organic pollutant residues, uses water as a medium and emits no VOCs, making it green and safe. At the same time, it improves the hydrophobicity of silk quilts and effectively reduces their moisture regain. The cashew nut shell phenol-blocked polyisocyanate prepared in this invention has strong hydrophobic properties, high molecular cohesive energy, and strong adhesion. Introducing it into the finishing solution can improve the adhesion of the finishing solution to the fiber and the film-forming flexibility. In addition, the cashew nut shell phenol-blocked polyisocyanate is a product in which the active isocyanate (-NCO) functional groups are temporarily blocked by cashew nut shell phenol (phenolic hydroxyl groups). After high-temperature baking heat treatment, it will release active isocyanate groups. These groups can react with the active hydrogen on the surface of silk fibers and cross-link with the amino groups of γ-aminopropyltriethoxysilane in the hydrophobic finishing agent to form a stable covalent network. This firmly anchors the hydrophobic polymer to the surface of silk fibers, significantly improving the wash resistance of silk quilts.

[0024] Compared with traditional technologies, this invention introduces branched amino silicone oil, whose active amino groups can undergo cross-linking reactions with the isocyanate groups released by cashew phenol-blocked polyisocyanates, jointly constructing an elastic network with cross-linking density. While enhancing water resistance, it can effectively maintain the natural texture of silk quilts, avoiding hardening or deformation caused by chemical treatment, so that the finished product remains soft and delicate. Detailed Implementation

[0025] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0026] It should be noted that there are no special restrictions on the manufacturers of the raw materials involved in this invention. Exemplarily, in this embodiment, the emulsifier is fatty alcohol polyoxyethylene ether (AEO-9), and the remaining raw materials are all commercially available.

[0027] Example 1: A method for preparing a washable, low-moisture-regain silk quilt, comprising the following processes: Step S1: Add the hydrophobic finishing agent and cashew phenol blocked polyisocyanate to water, then add branched amino silicone oil, emulsifier and rosmarinic acid, stir evenly to obtain the finishing solution; the finishing solution consists of 30 g / L hydrophobic finishing agent, 10 g / L cashew phenol blocked polyisocyanate, 3 g / L branched amino silicone oil, 1.5 g / L emulsifier and 1 g / L rosmarinic acid; Step S2: Immerse the silk floss sheet in the finishing solution under vibration at a temperature of 30℃ for 1 hour; the bath ratio (by mass) is 1:10. Remove the sheet, wash it with water, dry it at 100℃ for 1 minute, and bake it at 150℃ for 50 seconds to obtain a washable silk floss sheet. Pull the washable silk floss sheet apart, lay it layer by layer, twist it, and fix it to obtain a silk quilt. Finally, perform quilting and positioning to obtain a washable, low-moisture silk quilt. The preparation method of the hydrophobic finishing agent is as follows: 10g of octadecaneamine and 1000g of deionized water were stirred evenly at 60℃ to obtain an octadecaneamine aqueous solution; 1000g of octadecaneamine aqueous solution and 1000g of 30wt% tetraethyl orthosilicate aqueous dispersion were stirred at room temperature for 10h, 20g of hexadecyltrimethoxysilane and 40g of methyltrimethoxysilane were added, and the mixture was stirred for 1h; finally, 20g of γ-aminopropyltriethoxysilane was added, and the mixture was stirred for 3h to obtain a hydrophobic finishing agent; The preparation method of cashew phenol blocked polyisocyanate is as follows: Cashew phenol NX-2023, isophorone diisocyanate, and ethyl acetate were mixed evenly and reacted at 80℃ for 7 hours. The reaction was detected by di-n-butylamine back titration until -NCO was no longer detectable. The solvent was recovered by vacuum distillation to obtain cashew phenol blocked polyisocyanate. The molar ratio of the phenolic hydroxyl group of cashew phenol to the -NCO of isophorone diisocyanate was 1.1:1. The preparation method of branched amino silicone oil is as follows: Step A: Mix 10g vinyldimethylsilanol and 5g N,N-dimethylformamide evenly, replace with nitrogen, add 2g 1,8-diazabicycloundec-7-ene, 20g toluene and 80g hexamethylcyclotrisiloxane, react at room temperature for 4h, add acetic acid to neutralize for 8min, wash with deionized water, remove water from the organic phase with anhydrous sodium sulfate, remove toluene and N,N-dimethylformamide under reduced pressure to obtain α-vinyl-ω-hydroxy polydimethylsiloxane; Step B: Mix 10g of α-vinyl-ω-hydroxy polydimethylsiloxane, 6g of aminoethylaminopropyltrimethoxysilane and 0.2g of 1,8-diazabicycloundec-7-ene evenly, under nitrogen protection, react at 70°C for 3h, and remove residual reactants at -0.095MPa and 150°C to obtain the intermediate; Step C: Mix 100g of hydroxyl-terminated polydimethylsiloxane and 9g of intermediate evenly, under nitrogen protection, heat to 75℃, add a mixed solution of 0.3g potassium hydroxide and 5g water, and react at -0.095MPa for 3h to obtain branched amino silicone oil.

[0028] Example 2: A method for preparing a washable, low-moisture-regain silk quilt, comprising the following processes: Step S1: Add the hydrophobic finishing agent and cashew phenol blocked polyisocyanate to water, then add branched amino silicone oil, emulsifier and rosmarinic acid, stir evenly to obtain the finishing solution; the finishing solution consists of 40 g / L hydrophobic finishing agent, 20 g / L cashew phenol blocked polyisocyanate, 4 g / L branched amino silicone oil, 2 g / L emulsifier and 1.5 g / L rosmarinic acid; Step S2: Immerse the silk floss sheet in the finishing solution under vibration at a temperature of 40℃ for 2 hours; the bath ratio (by mass) is 1:15. Remove the sheet, wash it with water, dry it at 105℃ for 1.5 minutes, and bake it at 155℃ for 60 seconds to obtain a washable silk floss sheet. Pull the washable silk floss sheet apart, lay it layer by layer, twist it, and fix it to obtain a silk quilt. Finally, perform quilting and positioning to obtain a washable, low-moisture silk quilt. The preparation method of the hydrophobic finishing agent is as follows: 10g of octadecaneamine and 1050g of deionized water were stirred evenly at 65℃ to obtain an octadecaneamine aqueous solution; 1000g of octadecaneamine aqueous solution and 1500g of 35wt% tetraethyl orthosilicate aqueous dispersion were stirred at room temperature for 11h, 24g of hexadecyltrimethoxysilane and 48g of methyltrimethoxysilane were added, and the mixture was stirred for 1.5h; finally, 24g of γ-aminopropyltriethoxysilane was added, and the mixture was stirred for 3.5h to obtain a hydrophobic finishing agent; The preparation method of cashew phenol blocked polyisocyanate is as follows: Cashew phenol NX-2026, toluene diisocyanate, and ethyl acetate were mixed evenly and reacted at 60℃ for 10 h. The reaction was detected by di-n-butylamine back titration until -NCO was no longer detectable. The solvent was recovered by vacuum distillation to obtain cashew phenol blocked polyisocyanate. The molar ratio of the phenolic hydroxyl group of cashew phenol to the -NCO of toluene diisocyanate was (1.1-1.3):1. The preparation method of branched amino silicone oil is as follows: Step A: Mix 10g vinyldimethylsilanol and 8g N,N-dimethylformamide evenly, replace with nitrogen, add 3g 1,8-diazabicycloundec-7-ene, 20g toluene and 90g hexamethylcyclotrisiloxane, react at room temperature for 5h, add acetic acid to neutralize for 9min, wash with deionized water, remove water from the organic phase with anhydrous sodium sulfate, remove toluene and N,N-dimethylformamide under reduced pressure to obtain α-vinyl-ω-hydroxy polydimethylsiloxane; Step B: Mix 10g of α-vinyl-ω-hydroxy polydimethylsiloxane, 7g of aminoethylaminopropyltrimethoxysilane and 0.25g of 1,8-diazabicycloundec-7-ene evenly, under nitrogen protection, react at 75°C for 4h, and remove residual reactants at -0.095MPa and 150°C to obtain the intermediate; Step C: Mix 100g of hydroxyl-terminated polydimethylsiloxane and 10g of intermediate evenly, under nitrogen protection, heat to 80℃, add a mixed solution of 0.4g potassium hydroxide and 7g water, and react at -0.095MPa for 3h to obtain branched amino silicone oil.

[0029] Example 3: A method for preparing a washable, low-moisture-regain silk quilt, comprising the following processes: Step S1: Add the hydrophobic finishing agent and cashew phenol blocked polyisocyanate to water, then add branched amino silicone oil, emulsifier and rosmarinic acid, stir evenly to obtain the finishing solution; the finishing solution consists of 50 g / L hydrophobic finishing agent, 30 g / L cashew phenol blocked polyisocyanate, 5 g / L branched amino silicone oil, 3 g / L emulsifier and 2 g / L rosmarinic acid; Step S2: Immerse the silk floss sheet in the finishing solution under vibration at a temperature of 50℃ for 3 hours; the bath ratio (by mass) is 1:20. Remove the sheet, wash it with water, dry it at 110℃ for 2 minutes, and bake it at 160℃ for 70 seconds to obtain a washable silk floss sheet. Pull the washable silk floss sheet apart, lay it layer by layer, twist it, and fix it to obtain a silk quilt. Finally, perform quilting and positioning to obtain a washable, low-moisture silk quilt. The preparation method of the hydrophobic finishing agent is as follows: 10g of octadecaneamine and 1100g of deionized water were stirred evenly at 70℃ to obtain an octadecaneamine aqueous solution; 1000g of octadecaneamine aqueous solution and 2000g of 40wt% tetraethyl orthosilicate aqueous dispersion were stirred at room temperature for 12h, 30g of hexadecyltrimethoxysilane and 40g of methyltrimethoxysilane were added, and the mixture was stirred for 2h; finally, 20g of γ-aminopropyltriethoxysilane was added, and the mixture was stirred for 4h to obtain a hydrophobic finishing agent; The preparation method of cashew phenol blocked polyisocyanate is as follows: Cashew phenol NX-2025, diphenylmethane diisocyanate, and ethyl acetate were mixed evenly and reacted at 70°C for 8 hours. The reaction was detected by di-n-butylamine back titration until -NCO was no longer detectable. The solvent was recovered by vacuum distillation to obtain cashew phenol blocked polyisocyanate. The molar ratio of the phenolic hydroxyl group of cashew phenol to the -NCO of diphenylmethane diisocyanate was 1.3:1.

[0030] The preparation method of branched amino silicone oil is as follows: Step A: Mix 10g vinyldimethylsilanol and 10g N,N-dimethylformamide evenly, replace with nitrogen, add 4g 1,8-diazabicycloundec-7-ene, 40g toluene and 100g hexamethylcyclotrisiloxane, react at room temperature for 6h, add acetic acid to neutralize for 10min, wash with deionized water, remove water from the organic phase with anhydrous sodium sulfate, remove toluene and N,N-dimethylformamide under reduced pressure to obtain α-vinyl-ω-hydroxy polydimethylsiloxane; Step B: Mix 10g of α-vinyl-ω-hydroxy polydimethylsiloxane, 8g of aminoethylaminopropyltrimethoxysilane and 0.3g of 1,8-diazabicycloundec-7-ene evenly, under nitrogen protection, react at 80℃ for 5h, and remove residual reactants at -0.095MPa and 150℃ to obtain the intermediate; Step C: Mix 100g of hydroxyl-terminated polydimethylsiloxane and 12g of intermediate evenly, under nitrogen protection, heat to 85℃, add a mixed solution of 0.5g potassium hydroxide and 8g water, and react at -0.095MPa for 4h to obtain branched amino silicone oil.

[0031] Comparative Example 1: Comparative Example 1 is based on Example 2. However, cashew phenol-blocked polyisocyanate was not introduced into the finishing solution of Comparative Example 1. The remaining process steps and reaction parameters were the same as in Example 2. The specific differences are as follows: A method for preparing a washable, low-moisture-regain silk quilt includes the following processes: Step S1: Add the hydrophobic finishing agent to water, then add branched amino silicone oil, emulsifier and rosmarinic acid, stir evenly to obtain the finishing solution; the finishing solution consists of 40 g / L hydrophobic finishing agent, 4 g / L branched amino silicone oil, 2 g / L emulsifier and 1.5 g / L rosmarinic acid; Step S2: Immerse the silk floss sheet in the finishing solution under vibration at a temperature of 40℃ for 2 hours; the bath ratio (by mass) is 1:15. Remove the sheet, wash it with water, dry it at 105℃ for 1.5 minutes, and bake it at 155℃ for 60 seconds to obtain a washable silk floss sheet. Pull the washable silk floss sheet apart, lay it layer by layer, twist it, and fix it to obtain a silk quilt. Finally, perform quilting and positioning to obtain a washable, low-moisture silk quilt.

[0032] Comparative Example 2: Comparative Example 2 is based on Example 2. No hydrophobic finishing agent was introduced into the finishing solution of Comparative Example 2. The remaining process steps and reaction parameters were the same as in Example 2. Specific differences are as follows: A method for preparing a washable, low-moisture-regain silk quilt includes the following processes: Step S1: Add cashew phenol blocked polyisocyanate to water, then add branched amino silicone oil, emulsifier and rosmarinic acid, stir evenly to obtain finishing solution; the finishing solution is composed of 20 g / L cashew phenol blocked polyisocyanate, 4 g / L branched amino silicone oil, 2 g / L emulsifier and 1.5 g / L rosmarinic acid. Step S2: Immerse the silk floss sheet in the finishing solution under vibration at a temperature of 40℃ for 2 hours; the bath ratio (by mass) is 1:15. Remove the sheet, wash it with water, dry it at 105℃ for 1.5 minutes, and bake it at 155℃ for 60 seconds to obtain a washable silk floss sheet. Pull the washable silk floss sheet apart, lay it layer by layer, twist it, and fix it to obtain a silk quilt. Finally, perform quilting and positioning to obtain a washable, low-moisture silk quilt.

[0033] Comparative Example 3: Comparative Example 3 is based on Example 2, except that the branched amino silicone oil is replaced with the same mass of linear amino silicone oil. The remaining process steps and reaction parameters are the same as in Example 2. The specific differences are as follows: A method for preparing a washable, low-moisture-regain silk quilt includes the following processes: Step S1: Add the hydrophobic finishing agent and cashew phenol blocked polyisocyanate to water, then add linear amino silicone oil, emulsifier and rosmarinic acid, stir evenly to obtain the finishing solution; the finishing solution consists of 40 g / L hydrophobic finishing agent, 20 g / L cashew phenol blocked polyisocyanate, 4 g / L linear amino silicone oil, 2 g / L emulsifier and 1.5 g / L rosmarinic acid; Step S2: Immerse the silk floss sheet in the finishing solution under vibration at a temperature of 40℃ for 2 hours; the bath ratio (by mass) is 1:15. Remove the sheet, wash it with water, dry it at 105℃ for 1.5 minutes, and bake it at 155℃ for 60 seconds to obtain a washable silk floss sheet. Pull the washable silk floss sheet apart, lay it layer by layer, twist it, and fix it to obtain a silk quilt. Finally, perform quilting and positioning to obtain a washable, low-moisture silk quilt.

[0034] Experiment: Water-resistant washable silk floss sheets obtained in Examples 1-3 and Comparative Examples 1-3 were used to prepare samples. Their properties were tested and the test results were recorded. Water contact angle test: Place the silk fabric on the contact angle measuring instrument to measure its water contact angle, with a drop volume of 3μL.

[0035] Washability test: The fabric is immersed in 4g / L soap solution with a liquor ratio of 1:50, placed in a wash fastness tester and shaken for 5 minutes at 45℃. After washing, it is washed with cold water and then dried, which completes one wash. After 50 washes, the water contact angle is measured again, which is the main evaluation index of washability.

[0036] Referring to GB / T 9995 for determining moisture regain, the sample is conditioned for 24 hours under standard atmospheric conditions of 20±2℃ and 65±4% relative humidity to achieve moisture equilibrium. The conditioned sample is then quickly placed into a pre-weighed weighing bottle and weighed, recording the wet weight (including the weighing bottle). The weighing bottle containing the sample is then placed in an oven preheated to 140±2℃ for 2 hours. After drying, the bottle is capped, removed, and quickly transferred to a desiccator. It is then cooled to room temperature and weighed again. The sample is then placed back into the oven and dried for another 30 minutes, removed, cooled, and weighed. If the difference between two consecutive weighings is ≤0.05%, it is considered to have reached constant weight, and the final dry weight (including the weighing bottle) is recorded. If constant weight is not reached, drying continues until constant weight is achieved, and the moisture regain is calculated.

[0037] The test results are shown in Table 1.

[0038] Table 1

[0039] Based on the data in the table above, the following conclusions can be clearly drawn: Based on Examples 1-3 and Comparative Examples 1-3, it can be seen that the water-resistant filament sheet prepared by the present invention has excellent water-resistant properties and low moisture regain.

[0040] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.

Claims

1. A method for preparing a washable, low-moisture-regain silk quilt, characterized in that: Includes the following steps: Step S1: Add the hydrophobic finishing agent and cashew phenol blocked polyisocyanate to water, then add branched amino silicone oil, emulsifier and rosmarinic acid, stir evenly to obtain the finishing solution; Step S2: Immerse the silk floss sheet in the finishing solution, take it out, wash it, dry it, and bake it to obtain a washable silk floss sheet; stretch the washable silk floss sheet, lay it layer by layer, twist it, and fix it to obtain a silk quilt; finally, perform quilting and positioning to obtain a washable, low-moisture silk quilt.

2. The method for preparing a washable, low-moisture-regain silk quilt according to claim 1, characterized in that: The finishing solution consists of 30-50 g / L hydrophobic finishing agent, 10-30 g / L cashew phenol blocked polyisocyanate, 3-5 g / L branched amino silicone oil, 1.5-3.0 g / L emulsifier, and 1-2 g / L rosmarinic acid.

3. The method for preparing a washable, low-moisture-regain silk quilt according to claim 1, characterized in that: The preparation method of the hydrophobic finishing agent is as follows: Octadecylamine and deionized water were stirred evenly at 60-70℃ to obtain an aqueous solution of octadecylamine; the aqueous solution of octadecylamine and an aqueous dispersion of tetraethyl orthosilicate were stirred at room temperature for 10-12 h, hexadecyltrimethoxysilane and methyltrimethoxysilane were added, and the mixture was stirred for 1-2 h; finally, γ-aminopropyltriethoxysilane was added, and the mixture was stirred for 3-4 h to obtain a hydrophobic finishing agent.

4. The method for preparing a washable, low-moisture-regain silk quilt according to claim 3, characterized in that: The mass ratio of the aqueous solution of hexadecyltrimethoxysilane, methyltrimethoxysilane, γ-aminopropyltriethoxysilane and octadecylamine is (1-1.5):2:1:

50.

5. The method for preparing a washable, low-moisture-regain silk quilt according to claim 1, characterized in that: The method for preparing the cashew phenol blocked polyisocyanate is as follows: Cashew nut phenol, polyisocyanate and ethyl acetate are mixed evenly and reacted at 60-90℃ for 7-10 hours until -NCO is no longer detectable. The solvent is then recovered by vacuum distillation to obtain cashew nut phenol blocked polyisocyanate.

6. The method for preparing a washable, low-moisture-regain silk quilt according to claim 5, characterized in that: The molar ratio of the phenolic hydroxyl group of the cashew phenol to the -NCO of the polyisocyanate is (1.1-1.3):

1.

7. The method for preparing a washable, low-moisture-regain silk quilt according to claim 1, characterized in that: The preparation method of the branched amino silicone oil is as follows: Step A: Mix vinyl dimethylsilanol and N,N-dimethylformamide evenly, replace with nitrogen, add 1,8-diazabicycloundec-7-ene, toluene and hexamethylcyclotrisiloxane, react at room temperature for 4-6 h, add acetic acid to neutralize for 8-10 min, wash with deionized water, remove water from the organic phase with anhydrous sodium sulfate, remove toluene and N,N-dimethylformamide under reduced pressure to obtain α-vinyl-ω-hydroxy polydimethylsiloxane; Step B: Mix α-vinyl-ω-hydroxy polydimethylsiloxane, aminoethylaminopropyltrimethoxysilane and 1,8-diazabicycloundec-7-ene evenly, under nitrogen protection, and react at 70-80℃ for 3-5h. Remove residual reactants at -0.095MPa and 150℃ to obtain the intermediate. Step C: Mix hydroxyl-terminated polydimethylsiloxane and intermediate evenly, under nitrogen protection, heat to 75-85℃, add a mixed solution of potassium hydroxide and water, and react at -0.095MPa for 3-4 hours to obtain branched amino silicone oil.

8. The method for preparing a washable, low-moisture-regain silk quilt according to claim 7, characterized in that: In step C, the mass ratio of the hydroxyl-terminated polydimethylsiloxane, the intermediate, potassium hydroxide, and water is 100:(9-12):(0.003-0.005):(0.05-0.08).

9. The method for preparing a washable, low-moisture-regain silk quilt according to claim 1, characterized in that: The drying temperature is 100-110℃ and the time is 1-2 minutes; the baking temperature is 150-160℃ and the time is 50-70 seconds.

10. A washable, low-moisture-regain silk quilt prepared by the preparation method according to any one of claims 1-9.

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