Preparation method of waterproof moisture-permeable film for outdoor clothes

By combining polymer resin, maleic anhydride grafted chitosan, modified high-nano-based bentonite and phase-change temperature-regulating microcapsules, electrospinning technology is used to prepare outdoor clothing waterproof and moisture-permeable films, which solves the problem that the existing waterproof and moisture-permeable films cannot adjust the temperature, and achieves intelligent temperature control and efficient waterproof and moisture-permeable effect.

CN119980570AActive Publication Date: 2025-05-13HUAMAO (XIAMEN) WEAVING DYEING & FINISHING CO LTD
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Patent Information

Application Number
CN202510353548.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-25
Publication Date
2025-05-13
Estimated Expiration
2045-03-25

AI Technical Summary

Technical Problem

The existing waterproof and moisture-permeable membrane cannot be actively adjusted according to the weather environment or the human body temperature during use, which affects the high-end wearing experience.

Method used

By combining polymer resin, maleic anhydride grafted chitosan, modified high-nanobase bentonite and phase-change temperature-regulating microcapsules, outdoor clothing waterproof and moisture-permeable film is prepared by electrospinning technology to achieve intelligent temperature control effect.

Benefits of technology

It realizes intelligent temperature control with body temperature changes, improves the hydrostatic pressure protection capability of the waterproof and moisture-permeable film, enhances the temperature regulation effect, and avoids the damage to the human body by temperature difference.

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Abstract

The invention discloses a preparation method of a waterproof moisture-permeable film for outdoor clothing, and relates to the technical field of clothing, and the preparation method comprises the following steps: step 1, preparing a spinning solution: mixing and stirring polymer resin and a solvent, and preparing to obtain the spinning solution; 2, electrostatic spinning, wherein the spinning solution prepared in the step 1 is guided into an electrostatic spinning machine, and a waterproof moisture-permeable film blank is obtained through the spinning procedure; wherein the polymer resin comprises TPU (Thermoplastic Polyurethane) or PU (Polyurethane), maleic anhydride grafted chitosan and / or modified high-sodium bentonite and phase-change temperature-regulating microcapsules, the mass ratio of the maleic anhydride grafted chitosan and / or modified high-sodium bentonite to the polymer resin is 3-12%, and the mass ratio of the phase-change temperature-regulating microcapsules to the polymer resin is 20-42%. By combining the maleic anhydride grafted chitosan and the phase-change temperature-adjusting microcapsules, the compatibility of the phase-change temperature-adjusting microcapsules in the polymer resin is improved, the phase-change temperature-adjusting microcapsules are uniformly dispersed in the polymer resin, and the effect of efficient intelligent temperature control is achieved.
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Description

Technical Field

[0001] The present application relates to the technical field of clothing and accessories, and in particular to a method for preparing a waterproof and breathable membrane for outdoor clothing. Background Art

[0002] Electrospinning, also known as "electrospinning", is a processing method that makes a charged polymer solution or melt jet in an electrostatic field to prepare polymer ultrafine fibers.

[0003] The electrospinning device is simple in composition, consisting of a high-voltage power supply, a propulsion pump, a syringe, a needle and a collector. During electrospinning, the positive electrode of the high-voltage power supply is connected to the needle, and the negative electrode is connected to the collector and grounded. During electrospinning, the solution or melt droplets are pushed out of the needle by the syringe and the propulsion pump, and are charged under high voltage, and then stretched into fibers and collected by the collector. The specific principle is: under the action of high voltage electricity, the surface of the polymer solution or melt will be charged, forming an electrostatic repulsion opposite to the surface tension. When the electric field strength exceeds the critical value, the capillary filaments formed by the droplets are stretched to form a cone, namely the "Taylor cone". A fine jet will be formed at the bottom of the Taylor cone. Due to the bending instability, the jet will perform a violent whipping motion after moving a short distance in a straight line. Accompanied by the volatilization of the solvent, the jet forms extremely fine fibers and is deposited on the surface of the collector.

[0004] A Chinese patent with announcement number CN113123128B discloses a waterproof and breathable membrane, a preparation method and application thereof. The waterproof and breathable membrane includes a fiber matrix and a hydrophobic layer cross-linked with the fiber matrix. The preparation method of the waterproof and breathable membrane includes the following steps: S1: dissolving a hydrophilic polymer and a blocked solvent isocyanate in a solvent to obtain an electrospinning solution, and preparing a fiber matrix by electrospinning; S2: immersing the fiber matrix prepared in step S1 in a waterproofing agent solution and then drying it.

[0005] However, the durability of the waterproof and breathable membrane is improved only by fixing the waterproof agent on the surface of the polymer fiber, which makes it impossible to actively adjust the human body temperature according to the weather environment during use, affecting the high-end wearing experience and needs to be improved. Summary of the invention

[0006] In view of this, the purpose of this application is to provide a method for preparing a waterproof and breathable membrane for outdoor clothing to achieve the purpose of intelligent temperature control with changes in body temperature. The specific scheme is as follows:

[0007] A method for preparing a waterproof and breathable membrane for outdoor clothing comprises the following steps:

[0008] Step 1, spinning solution preparation: mixing and stirring the polymer resin and the solvent to obtain the spinning solution;

[0009] Step 2, electrospinning: introducing the spinning solution obtained in step 1 into an electrospinning machine, and obtaining a waterproof and breathable membrane embryo through a spinning process;

[0010] Wherein, the polymer resin includes TPU or PU, maleic anhydride grafted chitosan and / or modified high-nano bentonite and phase change temperature regulating microcapsules, and the mass ratio of the maleic anhydride grafted chitosan and / or modified high-nano bentonite to the polymer resin is 3-12%, and the mass ratio of the phase change temperature regulating microcapsules to the polymer resin is 20-42%.

[0011] Preferably: the preparation method of maleic anhydride grafted chitosan comprises the steps of ① chitosan activation: dissolving chitosan in a 1% glacial acetic acid solution to obtain a chitosan / glacial acetic acid solution with a mass concentration of 2.5%; ② grafting solution preparation: dissolving 2,3-diphenylmaleic anhydride in an acetone solution to obtain a grafting solution with a concentration of 0.48 g / ml; ③ grafting reaction: pouring the grafting solution into the chitosan / glacial acetic acid solution, stirring and reacting for 3-5 hours to obtain a grafting reaction solution; and ④ washing and discharging: adding an alkaline liquid to the grafting reaction solution, adjusting the pH to 9 and obtaining a precipitate, and washing the precipitate with ethanol / acetone in turn, and drying to obtain a finished maleic anhydride grafted chitosan.

[0012] Preferably: in step ③, 0.025 g / ml of ammonium cerium nitrate is added to the chitosan / glacial acetic acid solution as a catalyst, and the reaction is controlled in an inert gas at a temperature of 90°C.

[0013] Preferably: in step ③, the molar ratio of chitosan in the chitosan / glacial acetic acid solution to 2,3-diphenylmaleic anhydride in the grafting solution is 1:2.

[0014] Preferably: in step ④, the alkaline liquid is 1 mol / L sodium hydroxide solution.

[0015] Preferably: the modified high nano-bentonite is purchased from Wuhu Shuohua New Material Technology Co., Ltd., and has a bulk density of 0.61 g / ml.

[0016] Preferably, the mass ratio of the maleic anhydride grafted chitosan to the modified high sodium bentonite is 5:1-2.

[0017] Preferably: the phase change temperature regulating microcapsules have a phase change enthalpy value of ≥170 J / g and are purchased from PCM of Forsman.

[0018] Preferably: in step 2, the direct current spinning voltage of the electrospinning is 12-25 kV, the spinning solution propulsion perfusion speed is 1.0-2.4 mL / h, and the receiving distance is 8-15 cm.

[0019] Preferably, the electrospinning solvent is N,N-dimethylformamide or N,N-dimethylacetamide and acetone in a volume ratio of 1:2.2-2.8, and the mass fraction of the polymer in the spinning solution is 12-20%.

[0020] It can be seen from the above scheme that the present application provides a method for preparing a waterproof and breathable membrane for outdoor clothing, and the method for preparing a waterproof and breathable membrane for outdoor clothing has the following beneficial effects:

[0021] 1. By combining maleic anhydride grafted chitosan with phase change temperature regulating microcapsules, the compatibility of phase change temperature regulating microcapsules in polymer resin is improved and evenly dispersed in the polymer resin, achieving the effect of efficient and intelligent temperature control;

[0022] 2. When the phase-change temperature-regulating microcapsules are mixed with the polymer resin and dispersed in the solvent, the surface tension of the constituent materials is significantly reduced by combining maleic anhydride-grafted chitosan and modified high-nano bentonite, thereby effectively improving the hydrostatic pressure protection capability of the outdoor clothing waterproof and breathable membrane prepared by the preparation method of the outdoor clothing waterproof and breathable membrane;

[0023] 3. The maleic anhydride grafted chitosan obtained by grafting 2,3-diphenylmaleic anhydride with chitosan has effective compatibility with polymer resin and solvent, thereby obtaining a uniformly dispersed spinning solution;

[0024] 4. The function of phase-change thermostatic microcapsules is used to reduce human body temperature fluctuations, thereby avoiding damage to the human body caused by excessive temperature differences. TPU or PU, maleic anhydride grafted chitosan and / or modified high-nano bentonite are combined with phase-change thermostatic microcapsules through electrostatic spinning to obtain moisture permeability, air permeability and the effect of enabling the phase-change thermostatic microcapsules to play a regulating role in the pores of the waterproof and breathable membrane of outdoor clothing;

[0025] 5. Achieve intelligent temperature control according to changes in body temperature. DETAILED DESCRIPTION

[0026] The following will be clearly and completely described in conjunction with the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0027] It should be mentioned that the phase change thermostatic microcapsules in the embodiments of the present application are PCM purchased from Forsman and have a phase change enthalpy value of ≥170 J / g. The modified high nano-bentonite was purchased from Wuhu Shuohua New Materials Technology Co., Ltd. and has a bulk density of 0.61 g / ml. The remaining materials are commercially available and will not be described in detail here.

[0028] The following is a detailed description of the method for preparing the waterproof and breathable membrane for outdoor clothing of the present application.

[0029] A method for preparing a waterproof and breathable membrane for outdoor clothing comprises the following steps:

[0030] Step 1, spinning solution preparation: mixing and stirring the polymer resin and the solvent to prepare the spinning solution, wherein the solvent is N,N-dimethylformamide or N,N-dimethylacetamide and acetone in a volume ratio of 1:2.2-2.8, and the mass fraction of the polymer in the spinning solution is 12-20%;

[0031] Step 2, electrospinning: the spinning solution obtained in step 1 is introduced into the electrospinning machine, the DC spinning voltage of the electrospinning is controlled to be 12-25 kV, the spinning solution propulsion injection speed is 1.0-2.4 mL / h, the receiving distance is 8-15 cm, and the waterproof and breathable membrane embryo is obtained through the spinning process.

[0032] The polymer resin includes TPU or PU, maleic anhydride grafted chitosan and / or modified high-nano bentonite and phase change temperature regulating microcapsules, and the mass ratio of maleic anhydride grafted chitosan and / or modified high-nano bentonite to the polymer resin is 3-12%, and the mass ratio of phase change temperature regulating microcapsules to the polymer resin is 20-42%.

[0033] It should be noted that the preparation method of maleic anhydride grafted chitosan includes the steps of ① chitosan activation: dissolving chitosan in a 1% glacial acetic acid solution to obtain a chitosan / glacial acetic acid solution with a mass concentration of 2.5%; ② grafting solution preparation: dissolving 2,3-diphenylmaleic anhydride in an acetone solution to obtain a grafting solution with a concentration of 0.48 g / ml; ③ grafting reaction: pouring the grafting solution into the chitosan / glacial acetic acid solution, stirring and reacting for 3-5 hours to obtain a grafting reaction solution; and ④ washing and discharging: adding an alkaline liquid to the grafting reaction solution, adjusting the pH to 9 and obtaining a precipitate, and washing the precipitate with ethanol / acetone and drying it in turn to obtain a finished maleic anhydride grafted chitosan.

[0034] In order to improve the efficiency of the grafting reaction, in step ③, 0.025 g / ml of ammonium cerium nitrate was added to the chitosan / glacial acetic acid solution as a catalyst, and the reaction was controlled to be inert gas and the temperature was 90° C. At the same time, during the grafting reaction, the molar ratio of chitosan in the chitosan / glacial acetic acid solution to 2,3-diphenylmaleic anhydride in the grafting solution was controlled to be 1:2.

[0035] In the embodiment of the present application, the alkaline liquid is 1 mol / L sodium hydroxide solution.

[0036] It should be mentioned that in order to improve the temperature regulation effect of the outdoor clothing waterproof and breathable membrane prepared by the preparation method of the outdoor clothing waterproof and breathable membrane, the mass ratio of maleic anhydride grafted chitosan and modified high sodium bentonite is 5:1-2.

[0037] Embodiment 1

[0038] A method for preparing a waterproof and breathable membrane for outdoor clothing comprises the following steps:

[0039] Step 1, spinning solution preparation: the polymer resin and the solvent are mixed and stirred to prepare the spinning solution, wherein the solvent is N,N-dimethylformamide and acetone in a volume ratio of 1:2.2, and the mass fraction of the polymer in the spinning solution is 12%;

[0040] Step 2, electrospinning: The spinning solution obtained in step 1 is introduced into the electrospinning machine, the DC spinning voltage of the electrospinning is controlled to be 12 kV, the spinning solution propulsion injection speed is 1.0 mL / h, the receiving distance is 8 cm, and the waterproof and breathable membrane embryo is obtained through the spinning process.

[0041] The polymer resin includes TPU, maleic anhydride grafted chitosan and phase change temperature regulating microcapsules, and the mass ratio of maleic anhydride grafted chitosan to the polymer resin is 3%, and the mass ratio of phase change temperature regulating microcapsules to the polymer resin is 20%.

[0042] It should be noted that the preparation method of maleic anhydride grafted chitosan includes the steps of ① chitosan activation: dissolving chitosan in a 1% glacial acetic acid solution to obtain a chitosan / glacial acetic acid solution with a mass concentration of 2.5%; ② grafting solution preparation: dissolving 2,3-diphenylmaleic anhydride in an acetone solution to obtain a grafting solution with a concentration of 0.48 g / ml; ③ grafting reaction: pouring the grafting solution into the chitosan / glacial acetic acid solution, and obtaining a grafting reaction solution after stirring and reacting for 3 hours; and ④ washing and discharging: adding an alkaline liquid to the grafting reaction solution, adjusting the pH to 9 and obtaining a precipitate, and successively washing the precipitate with ethanol / acetone and drying it to obtain a finished maleic anhydride grafted chitosan.

[0043] In order to improve the efficiency of the grafting reaction, in step ③, 0.025 g / ml of ammonium cerium nitrate was added to the chitosan / glacial acetic acid solution as a catalyst, and the reaction was controlled to be inert gas and the temperature was 90° C. At the same time, during the grafting reaction, the molar ratio of chitosan in the chitosan / glacial acetic acid solution to 2,3-diphenylmaleic anhydride in the grafting solution was controlled to be 1:2.

[0044] In the embodiment of the present application, the alkaline liquid is 1 mol / L sodium hydroxide solution.

[0045] Embodiment 2

[0046] A method for preparing a waterproof and breathable membrane for outdoor clothing comprises the following steps:

[0047] Step 1, spinning solution preparation: the polymer resin and the solvent are mixed and stirred to prepare the spinning solution, wherein the solvent is N,N-dimethylacetamide and acetone in a volume ratio of 1:2.5, and the mass fraction of the polymer in the spinning solution is 15%;

[0048] Step 2, electrospinning: The spinning solution obtained in step 1 is introduced into the electrospinning machine, the DC spinning voltage of the electrospinning is controlled to be 20 kV, the spinning solution propulsion injection speed is 1.6 mL / h, the receiving distance is 12 cm, and the waterproof and breathable membrane embryo is obtained through the spinning process.

[0049] The polymer resin includes TPU, maleic anhydride grafted chitosan, modified high sodium bentonite and phase change temperature regulating microcapsules, and the mass ratio of maleic anhydride grafted chitosan and modified high sodium bentonite to the polymer resin is 6%, and the mass ratio of phase change temperature regulating microcapsules to the polymer resin is 30%.

[0050] It should be noted that the preparation method of maleic anhydride grafted chitosan includes the steps of ① chitosan activation: dissolving chitosan in a 1% glacial acetic acid solution to obtain a chitosan / glacial acetic acid solution with a mass concentration of 2.5%; step ② grafting solution preparation: dissolving 2,3-diphenylmaleic anhydride in an acetone solution to obtain a grafting solution with a concentration of 0.48 g / ml; step ③ grafting reaction: pouring the grafting solution into the chitosan / glacial acetic acid solution, and obtaining a grafting reaction solution after stirring and reacting for 4 hours; step ④ washing and discharging: adding an alkaline liquid to the grafting reaction solution, and adjusting the pH to 9 to obtain a precipitate, and successively washing the precipitate with ethanol / acetone and drying it to obtain a finished maleic anhydride grafted chitosan.

[0051] In order to improve the efficiency of the grafting reaction, in step ③, 0.025 g / ml of ammonium cerium nitrate was added to the chitosan / glacial acetic acid solution as a catalyst, and the reaction was controlled to be inert gas and the temperature was 90° C. At the same time, during the grafting reaction, the molar ratio of chitosan in the chitosan / glacial acetic acid solution to 2,3-diphenylmaleic anhydride in the grafting solution was controlled to be 1:2.

[0052] In the embodiment of the present application, the alkaline liquid is 1 mol / L sodium hydroxide solution.

[0053] It should be mentioned that in order to improve the temperature regulating effect of the outdoor clothing waterproof and breathable membrane prepared by the preparation method of the outdoor clothing waterproof and breathable membrane, the mass ratio of maleic anhydride grafted chitosan and modified high sodium bentonite is 5:1.

[0054] Embodiment 3

[0055] A method for preparing a waterproof and breathable membrane for outdoor clothing comprises the following steps:

[0056] Step 1, spinning solution preparation: the polymer resin and the solvent are mixed and stirred to prepare the spinning solution, wherein the solvent is N,N-dimethylformamide and acetone in a volume ratio of 1:2.8, and the mass fraction of the polymer in the spinning solution is 20%;

[0057] Step 2, electrospinning: The spinning solution obtained in step 1 is introduced into the electrospinning machine, the DC spinning voltage of the electrospinning is controlled to be 25 kV, the spinning solution propulsion injection speed is 2.4 mL / h, the receiving distance is 15 cm, and the waterproof and breathable membrane embryo is obtained through the spinning process.

[0058] The polymer resin includes PU, maleic anhydride grafted chitosan, modified high sodium bentonite and phase change temperature regulating microcapsules, and the mass ratio of maleic anhydride grafted chitosan and modified high sodium bentonite to the polymer resin is 12%, and the mass ratio of phase change temperature regulating microcapsules to the polymer resin is 42%.

[0059] It should be noted that the preparation method of maleic anhydride grafted chitosan includes the steps of ① chitosan activation: dissolving chitosan in a 1% glacial acetic acid solution to obtain a chitosan / glacial acetic acid solution with a mass concentration of 2.5%; step ② grafting solution preparation: dissolving 2,3-diphenylmaleic anhydride in an acetone solution to obtain a grafting solution with a concentration of 0.48 g / ml; step ③ grafting reaction: pouring the grafting solution into the chitosan / glacial acetic acid solution, and obtaining a grafting reaction solution after stirring and reacting for 5 hours; step ④ washing and discharging: adding an alkaline liquid to the grafting reaction solution, and adjusting the pH to 9 to obtain a precipitate, and washing the precipitate with ethanol / acetone in turn, and drying to obtain a finished maleic anhydride grafted chitosan.

[0060] In order to improve the efficiency of the grafting reaction, in step ③, 0.025 g / ml of ammonium cerium nitrate was added to the chitosan / glacial acetic acid solution as a catalyst, and the reaction was controlled to be inert gas and the temperature was 90° C. At the same time, during the grafting reaction, the molar ratio of chitosan in the chitosan / glacial acetic acid solution to 2,3-diphenylmaleic anhydride in the grafting solution was controlled to be 1:2.

[0061] In the embodiment of the present application, the alkaline liquid is 1 mol / L sodium hydroxide solution.

[0062] It should be mentioned that in order to improve the temperature regulating effect of the outdoor clothing waterproof and breathable membrane prepared by the preparation method of the outdoor clothing waterproof and breathable membrane, the mass ratio of maleic anhydride grafted chitosan and modified high sodium bentonite is 5:2.

[0063] Comparative Example 1

[0064] The difference between Comparative Example 1 and Example 2 is that the maleic anhydride grafted chitosan in Comparative Example 1 is chitosan grafted with maleic anhydride, and the maleic anhydride is purchased from Jinan Huifengda Chemical Co., Ltd., and has a CAS number of 108-31-6.

[0065] Comparative Example 2

[0066] The difference between Comparative Example 2 and Example 2 is that in Comparative Example 2, activated chitosan is used instead of maleic anhydride grafted chitosan.

[0067] The difference between Comparative Example 3 and Example 2 is that no maleic anhydride grafted chitosan and modified high sodium bentonite are added in Comparative Example 3.

[0068] Performance Testing:

[0069] 1. Water pressure resistance test: GB / T 4744-2013 "Testing and evaluating the waterproof performance of textiles - Hydrostatic pressure method"

[0070] 2. Moisture permeability test: GB / T 32614-2016 "Outdoor sportswear jackets"

[0071] 3. Phase change enthalpy test: Differential scanning calorimetry (DSC)

[0072] The performance test results are shown in Table 1 and Table 2 below.

[0073] Table 1 Performance test results of embodiments and comparative examples

[0074]

[0075] Table 2 Performance test results of embodiment and comparative example 2

[0076] Phase change enthalpy (J / g) Embodiment 1 47 Embodiment 2 58 Embodiment 3 66 Comparative Example 1 50 Comparative Example 2 44 Comparative Example 3 35

[0077] As shown in Table 1 above, the synergistic effect of the maleic anhydride grafted chitosan and the phase change thermostatic microcapsules in the embodiment of the present application has the effect of effectively being compatible with the phase change thermostatic microcapsules, thereby stimulating the temperature control ability of the phase change thermostatic microcapsules to achieve the purpose of effective temperature control. As shown in Table 2 above, when the amount of the added phase change thermostatic microcapsules increases, the phase change enthalpy value of the outdoor clothing waterproof and breathable membrane has a significant positive effect, but when the amount of the phase change thermostatic microcapsules gradually increases, the increase in the phase change enthalpy value is no longer obvious, and the waterproof and breathable properties of the material will be affected. Therefore, it is necessary to effectively control the amount of the phase change thermostatic microcapsules, and make it cooperate with the maleic anhydride grafted chitosan and the modified high-nano bentonite to enhance the synergistic effect of each component in the spinning solution. Among them, the modified high-nano bentonite has the effect of improving adhesion and adsorption capacity, and then promoting the increase of the contact angle to reduce hydrophilicity and waterproofing.

[0078] In summary, the present application provides a method for preparing a waterproof and breathable film for outdoor clothing, which combines maleic anhydride grafted chitosan with phase change thermostatic microcapsules to improve the compatibility of phase change thermostatic microcapsules in polymer resins and evenly disperse them in polymer resins, thereby achieving the effect of efficient and intelligent temperature control. Among them, the maleic anhydride grafted chitosan obtained by grafting 2,3-diphenylmaleic anhydride and chitosan has effective compatibility with polymer resins and solvents, thereby obtaining a uniformly dispersed spinning solution, and when the phase change thermostatic microcapsules are mixed with the polymer resin and dispersed in the solvent, the maleic anhydride grafted chitosan and modified high-nano bentonite are combined to significantly reduce the surface tension of the constituent materials, thereby effectively improving the hydrostatic pressure protection capability of the waterproof and breathable film for outdoor clothing prepared by the method for preparing the waterproof and breathable film for outdoor clothing. At the same time, the waterproof and breathable membrane for outdoor clothing prepared by the method for preparing the waterproof and breathable membrane for outdoor clothing reduces the temperature fluctuation of the human body through the function of the phase-change temperature-regulating microcapsules, thereby avoiding the damage to the human body caused by excessive temperature difference, and obtains the effect of moisture permeability, air permeability and enabling the phase-change temperature-regulating microcapsules to play a regulating role in the pores of the waterproof and breathable membrane for outdoor clothing by combining TPU or PU, maleic anhydride grafted chitosan and / or modified high-nano bentonite with the phase-change temperature-regulating microcapsules through electrostatic spinning. Therefore, the method for preparing the waterproof and breathable membrane for outdoor clothing achieves the purpose of intelligent temperature control with changes in body temperature.

[0079] The "first", "second", "third", "fourth", etc. (if any) referred to in this application are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchangeable where appropriate, so that the embodiments described herein can be implemented in an order other than that described herein. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions, for example, a process, method or device comprising a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods or devices.

[0080] It should be noted that the descriptions involving "first", "second", etc. in this application are only for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the ability of ordinary technicians in this field to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by this application.

[0081] Specific examples are used herein to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method of the present application and its core idea. At the same time, for those skilled in the art, according to the idea of ​​the present application, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as a limitation on the present application.

Claims

1. A method for preparing a waterproof and breathable membrane for outdoor clothing, characterized in that: The steps include: Step 1, spinning solution preparation: mixing and stirring the polymer resin and the solvent to obtain the spinning solution; Step 2, electrospinning: introducing the spinning solution obtained in step 1 into an electrospinning machine, and obtaining a waterproof and breathable membrane embryo through a spinning process; Wherein, the polymer resin includes TPU or PU, maleic anhydride grafted chitosan and / or modified high-nano bentonite and phase change temperature regulating microcapsules, and the mass ratio of the maleic anhydride grafted chitosan and / or modified high-nano bentonite to the polymer resin is 3-12%, and the mass ratio of the phase change temperature regulating microcapsules to the polymer resin is 20-42%.

2. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 1, characterized in that: The preparation method of maleic anhydride grafted chitosan comprises the steps of: ① activating chitosan: dissolving chitosan in a 1% glacial acetic acid solution to obtain a chitosan / glacial acetic acid solution with a mass concentration of 2.5%; ② preparing a grafting solution: dissolving 2,3-diphenylmaleic anhydride in an acetone solution to obtain a grafting solution with a concentration of 0.48 g / ml; ③ grafting reaction: pouring the grafting solution into a chitosan / glacial acetic acid solution, stirring and reacting for 3-5 hours to obtain a grafting reaction solution; and ④ washing and discharging: adding an alkaline liquid into the grafting reaction solution, adjusting the pH to 9 and obtaining a precipitate, and washing the precipitate with ethanol / acetone in sequence, and drying the precipitate to obtain a finished maleic anhydride grafted chitosan.

3. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 2, characterized in that: In step ③, 0.025 g / ml of ammonium cerium nitrate is added to the chitosan / glacial acetic acid solution as a catalyst, and the reaction is controlled in an inert gas at a temperature of 90°C.

4. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 2, characterized in that: In step ③, the molar ratio of chitosan in the chitosan / glacial acetic acid solution to 2,3-diphenylmaleic anhydride in the grafting solution is 1:

2.

5. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 2, characterized in that: In step ④, the alkaline liquid is 1 mol / L sodium hydroxide solution.

6. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 1, characterized in that: The modified high nano-bentonite was purchased from Wuhu Shuohua New Material Technology Co., Ltd., and the bulk density was 0.61 g / ml.

7. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 6, characterized in that: The mass ratio of the maleic anhydride grafted chitosan to the modified high sodium bentonite is 5:1-2.

8. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 1, characterized in that: The phase change temperature regulating microcapsules have a phase change enthalpy value of ≥170 J / g and are purchased from PCM of Forsman.

9. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 1, characterized in that: In step 2, the direct current spinning voltage of the electrospinning is 12-25 kV, the spinning solution propulsion perfusion speed is 1.0-2.4 mL / h, and the receiving distance is 8-15 cm.

10. The method for preparing a waterproof and breathable membrane for outdoor clothing according to claim 9, characterized in that: The electrostatic spinning solvent is N,N-dimethylformamide or N,N-dimethylacetamide and acetone in a volume ratio of 1:2.2-2.8, and the mass fraction of the polymer in the spinning solution is 12-20%.

Citation Information

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