Temperature-adjusting textile based on phase-change microcapsules and preparation method of temperature-adjusting textile

The self-adhesive phase change microcapsules are prepared by electrospinning and monomer synthesis technology, and adhered to the textile by immersion, which solves the problems of complicated steps and weak adhesion in the prior art, and realizes the strong adhesion of the textile and excellent heat storage and temperature regulation function.

CN119615629AInactive Publication Date: 2025-03-14NINGBO MICRO NEW MATERIALS TECHNOLOGY CO LTD +1

Patent Information

Application Number
CN202411870940.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-18
Publication Date
2025-03-14
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing methods of organizing phase-change microcapsules into textiles are complicated, the process flow is complicated, and the adhesion of phase-change microcapsules is not strong and easy to lose.

Method used

Electrostatic spinning method is used to prepare nanofibers and natural fibers, and the wall material of phase-changing microcapsules is synthesized with 3-methacrylamide dopamine and methacrylic acid monomer. Paraffin wax is used as the core material to prepare phase-changing microcapsules with self-adhesion, and self-adhesive to the base fabric by immersion method.

Benefits of technology

It realizes strong adhesion of phase-change microcapsules on textiles, has mild process conditions, simple steps, and has excellent heat storage and temperature regulation function.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a temperature-adjusting textile based on phase-change microcapsules and a preparation method thereof, and belongs to the technical field of textiles, the method comprises the following steps: (1) preparing a polymer solution into nanofibers by using an electrostatic spinning method, and weaving the nanofibers and natural fiber blended yarns to obtain a basic fabric; (2) heating and melting paraffin, adding 3-methacrylamide dopamine and methacrylic acid, finally adding an initiator to prepare an oil-phase solution, pouring the oil-phase solution into a water-phase solution containing an emulsifier, stirring and emulsifying, and heating to generate polymerization reaction to obtain a phase change microcapsule; and (3) soaking the basic fabric in a solution containing the phase-change microcapsules to enable the phase-change microcapsules to be self-adhered to the basic fabric, taking out the basic fabric, padding, and drying to obtain the temperature-adjusting textile based on the phase-change microcapsules. The method is simple in steps, the phase change microcapsules are high in adhesive force on the basic fabric, and the obtained temperature adjusting textile has excellent heat storage and temperature adjusting functions.
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Description

Technical Field

[0001] The invention relates to the technical field of textiles, and in particular to a temperature-regulating textile based on phase-change microcapsules and a preparation method thereof. Background Art

[0002] With the development of science and technology and the gradual improvement of people's living standards, consumers' demand for textiles is no longer limited to basic functions such as warmth and covering, but pays more attention to its comfort, environmental protection and special functions (such as antibacterial, antistatic, temperature regulation, etc.). The research and development of functional textiles has gradually become the focus of the industry. Thermostatic textiles can automatically adjust the temperature according to the changes in human body temperature, solve the inconvenience caused by adding or removing clothes and the high energy consumption problem of adjusting the ambient temperature, and improve the comfort of the wearer.

[0003] Phase change materials (PCMs) have received special attention in the field of thermostatic textiles due to their excellent thermal management capabilities. PCMs are materials that can undergo phase changes within a specific temperature range. At the corresponding phase change temperature, they will undergo a corresponding phase change, absorbing or releasing a large amount of latent heat during the phase change process, thereby adjusting or controlling the ambient temperature of the thermostatic object. Phase change microcapsules (MPCPs) are phase change energy storage materials with a core-shell structure. Their working principle is to regulate temperature through the heat release and heat absorption process of phase change materials (the internal molecular form will transform between the crystalline region and the amorphous region).

[0004] The Chinese patent document with publication number CN117821025A discloses a phase change microcapsule and a preparation method thereof, wherein the method first uses magnetic stirring to prepare a surfactant dispersion system; then, emulsifying dispersant and phase change core material are sequentially added to the surfactant dispersion system, and dispersed using magnetic stirring to prepare a core material emulsified dispersion; then, a wall material suspension is prepared; finally, the wall material suspension is added dropwise to the core material emulsified dispersion system, and polymerized under magnetic stirring conditions to obtain a phase change microcapsule, wherein the process steps are simple and the obtained phase change microcapsule has few holes. The Chinese patent document with publication number CN107722943A discloses a preparation method of a paraffin phase change microcapsule, comprising: preparing a melamine modified urea formaldehyde resin prepolymer solution; adding paraffin and an emulsifier solution to the prepolymer solution to obtain a paraffin emulsion; adjusting the pH value of the paraffin emulsion to 3, and performing an in-situ polymerization reaction with constant temperature stirring to obtain a paraffin phase change microcapsule with a melamine modified urea formaldehyde resin as a wall material.

[0005] At present, the methods for finishing phase change microcapsules into textile materials include spinning method, coating finishing method and hollow fiber impregnation filling method, etc. For example, Chinese patent document with publication number CN116121893A discloses a microcapsule phase change temperature regulating lyocell fiber and its preparation method, which is prepared by solvent spinning of a mixed spinning solution consisting of aqueous cellulose with a moisture content of 10-60wt% after activation and squeezing treatment, an aqueous solution containing 50-88wt% N-methylmorpholine-N-oxide and a phase change emulsion containing 20-50wt% microcapsules; Chinese patent document with publication number CN104250934A discloses a microcapsule finishing method for maintaining the human body microenvironment, which prepares a mixed finishing solution of microcapsules A and phase change microcapsules B, attaches the mixed finishing solution to a first fabric, prepares a finishing solution of phase change microcapsules B, attaches the finishing solution of phase change microcapsules B to a second fabric, and finally sews the first fabric and the second fabric together, so that the finished fabric has both energy storage and temperature regulating functions.

[0006] However, the above method has complicated steps and a complex process flow. Summary of the invention

[0007] The invention provides a method for preparing a temperature-regulating textile based on phase-change microcapsules. The preparation conditions are mild and the steps are simple. The phase-change microcapsules are self-adhesive and have strong adhesion on the temperature-regulating textile and are not easy to be lost.

[0008] The specific technical solutions adopted are as follows:

[0009] A method for preparing a temperature-regulating textile based on phase-change microcapsules comprises the following steps:

[0010] (1) using electrospinning to prepare nanofibers from a polymer solution, and then spinning and weaving the nanofibers with natural fibers to obtain a basic fabric;

[0011] (2) After the paraffin is heated and melted, 3-methacrylamide dopamine and methacrylic acid are added, and finally an initiator is added to prepare an oil phase solution, and the oil phase solution is poured into an aqueous phase solution containing an emulsifier, stirred and emulsified, and heated to cause a polymerization reaction to obtain phase change microcapsules;

[0012] (3) Soaking the base fabric in a solution containing phase change microcapsules to allow the phase change microcapsules to self-adhere to the base fabric, taking it out, rolling it, and drying it to obtain the temperature-regulating textile based on phase change microcapsules.

[0013] The present invention firstly uses a polymer solution to prepare nanofibers. The nanofibers are easy to modify and have a large specific surface area. The diameter and morphology of the electrospun nanofibers are controllable, and the parameters of the electrospinning process can be adjusted according to specific usage requirements. Furthermore, the basic fabric obtained by blending the nanofibers with natural fibers for double-layer weaving has better mechanical properties and better adsorption properties. The present invention uses 3-methylacrylamide dopamine and methacrylic acid as monomers to synthesize the wall material of phase change microcapsules, and uses phase change material paraffin as a core material. The obtained phase change microcapsules have a self-adhesion function. The basic fabric is immersed in a solution containing the phase change microcapsules, so that the phase change microcapsules can self-adhere to the basic fabric with a strong binding force, thereby preparing the temperature-regulating textile based on phase change microcapsules.

[0014] Specifically, the polymer is a synthetic polymer, including but not limited to polyvinyl alcohol, nylon, polylactic acid or polyurethane; the natural fiber is any one of cotton and linen.

[0015] Preferably, in step (1), the concentration of the polymer solution is 13-20wt%; the parameters of the electrospinning process are: voltage 15-20kV, 15-20cm from the spinneret to the collector, flow rate 0.5-1.5mL / h, ambient temperature 20-30°C, ambient humidity 40%-50%. Under the above parameters, the electrospinning process is easy to carry out, and the uniformity of the obtained nanofibers is good.

[0016] Optionally, the mass ratio of nanofibers to natural fibers is 1:0.2-1.

[0017] The initiator includes but is not limited to azobisisobutyronitrile or benzoyl peroxide, and the added amount of the initiator accounts for 1wt% to 3wt% of the total mass of the two monomers of 3-methacrylamide dopamine and methacrylic acid.

[0018] Preferably, based on the total mass of the two monomers 3-methacrylamide dopamine and methacrylic acid, the mass ratio of paraffin to the two monomers is 1:0.1-1, further 1:0.5-1; the mass ratio of 3-methacrylamide dopamine to methacrylic acid is 1:1-2; 3-methacrylamide dopamine can be synthesized according to the records in the prior art or purchased.

[0019] The mass concentration of the emulsifier in the aqueous phase solution is 1wt% to 8wt%, and the emulsifier is sodium dodecylbenzene sulfonate, polyvinyl pyrrolidone or polysorbate monoether.

[0020] Preferably, the polymerization temperature is 60-90° C., and the polymerization reaction is carried out for 4-6 hours under mechanical stirring. Too short a polymerization reaction time will result in incomplete reaction, the capsule wall of some microcapsules is not strong, the capsule wall is easy to break, and the microcapsule encapsulation rate is low.

[0021] In step (3), the mass concentration of the phase change microcapsules in the solution containing the phase change microcapsules is 10wt% to 20wt%, and the immersion time is 30min to 2h.

[0022] The present invention also provides a temperature-regulating textile based on phase-change microcapsules prepared by the method for preparing the temperature-regulating textile based on phase-change microcapsules. The temperature-regulating textile based on phase-change microcapsules has an automatic temperature-regulating function.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] (1) The present invention uses 3-methacrylamide dopamine and methacrylic acid monomers to prepare the wall material of the phase change microcapsule, which not only has a high encapsulation rate, but also gives the phase change microcapsule self-adhesiveness, making it easy to arrange it on the textile material. The arrangement method is simple and does not require the addition of additional adhesives. In addition, the phase change microcapsule has strong adhesion on the textile and is not easy to lose, which has little effect on the performance of the textile.

[0025] (2) The present invention weaves a basic fabric by blending electrospun nanofibers and natural fibers. The basic fabric combines the advantages of electrospun nanofibers and natural fibers, has good air permeability, and is convenient for the adhesion of phase change microcapsules. The temperature-regulating textile based on phase change microcapsules provided by the present invention has excellent heat storage and temperature regulation functions. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 This is the SEM image of the phase change microcapsules prepared by the method in Example 1.

[0027] Figure 2 This is the SEM image of the phase change microcapsules prepared by the method in Example 2. DETAILED DESCRIPTION

[0028] In order to make the purpose, features and advantages of the present invention more obvious and easy to understand, the following is a detailed description through specific embodiments. In the following description, many specific details are set forth in order to fully understand the present invention. However, the present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without violating the connotation of the present invention, so the present invention is not limited by the specific embodiments disclosed below. The technical features in each embodiment of the present invention can be combined accordingly without conflicting with each other.

[0029] It should be noted that the following detailed descriptions are illustrative and are intended to provide further explanation of the present application. Unless otherwise specified, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which the present application belongs.

[0030] Example 1

[0031] (1) First, a 18 wt % nylon 66 formic acid solution was prepared and electrospun. The electrospinning process parameters were: voltage 18 kV, 15 cm from the spinneret to the collector, flow rate 1.0 mL / h, ambient temperature 28 ° C, ambient humidity 40% to 50%, and nanofibers were prepared. The nanofibers were blended with natural cotton fibers for weaving (the mass ratio of the nanofibers to the natural cotton fibers was 1:0.25) to obtain a basic fabric;

[0032] (2) After heating and melting paraffin, 3-methacrylamide dopamine and methacrylic acid are added, the mass ratio of 3-methacrylamide dopamine and methacrylic acid monomers is 1:1, and the total mass ratio of paraffin to 3-methacrylamide dopamine and methacrylic acid monomers is 1:0.5. Finally, an initiator azobisisobutyronitrile is added, and the amount of the initiator is 2wt% of the total mass of the 3-methacrylamide dopamine and methacrylic acid monomers to prepare an oil phase solution; a polyvinyl pyrrolidone aqueous solution with a mass concentration of 5wt% is used as an aqueous phase solution, and the oil phase solution is poured into the aqueous phase solution, and mechanically stirred at a speed of 1000r / min for emulsification for 10min; then, the temperature is raised to 80°C to carry out a polymerization reaction under mechanical stirring for 5h, and the solution after the reaction is solid-liquid separated, and the obtained solid is washed and dried to obtain phase change microcapsules;

[0033] (3) The base fabric is immersed in a solution containing 15 wt% of phase change microcapsules, and allowed to stand for 1 hour to allow the phase change microcapsules to self-adhere to the base fabric. After being taken out, the solution is rolled and dried to obtain the temperature-regulating textile based on phase change microcapsules.

[0034] Example 2

[0035] (1) First, a 20 wt% polyurethane organic solution (solvent N,N-dimethylformamide) was prepared and subjected to electrospinning. The electrospinning process parameters were: voltage 20 kV, 15 cm from spinneret to collector, flow rate 1.0 mL / h, ambient temperature 28° C., ambient humidity 40% to 50%, to prepare nanofibers, and the nanofibers were blended with natural cotton fibers for weaving (the mass ratio of the nanofibers to the natural cotton fibers was 1:0.2) to obtain a basic fabric;

[0036] (2) After heating and melting paraffin, 3-methacrylamide dopamine and methacrylic acid are added, the total mass ratio of paraffin to 3-methacrylamide dopamine and methacrylic acid monomers is 1:1, and the mass ratio of 3-methacrylamide dopamine to methacrylic acid monomers is 1:1. Finally, an initiator azobisisobutyronitrile is added, and the amount of the initiator is 2wt% of the total mass of the 3-methacrylamide dopamine and methacrylic acid monomers to prepare an oil phase solution; a polyvinyl pyrrolidone aqueous solution with a mass concentration of 5wt% is used as an aqueous phase solution, and the oil phase solution is poured into the aqueous phase solution, and mechanically stirred at a speed of 1000r / min for emulsification for 10min; then, the temperature is raised to 80°C to carry out a polymerization reaction under mechanical stirring for 5h, and the solution after the reaction is solid-liquid separated, and the obtained solid is washed and dried to obtain phase change microcapsules;

[0037] (3) The base fabric is immersed in a solution containing 20 wt% of phase change microcapsules, and allowed to stand for 1 hour to allow the phase change microcapsules to self-adhere to the base fabric. After being taken out, the solution is rolled and dried to obtain the temperature-regulating textile based on phase change microcapsules.

[0038] Example 3

[0039] (1) First, a 20 wt% polyurethane organic solution (solvent N,N-dimethylformamide) was prepared and subjected to electrospinning. The electrospinning process parameters were: voltage 20 kV, 15 cm from spinneret to collector, flow rate 1.0 mL / h, ambient temperature 28° C., ambient humidity 40% to 50%, to prepare nanofibers, and the nanofibers were blended with natural cotton fibers for weaving (the mass ratio of the nanofibers to the natural cotton fibers was 1:0.2) to obtain a basic fabric;

[0040] (2) After heating and melting paraffin, 3-methacrylamide dopamine and methacrylic acid are added, the total mass ratio of paraffin to 3-methacrylamide dopamine and methacrylic acid monomers is 1:0.5, and the mass ratio of 3-methacrylamide dopamine to methacrylic acid monomers is 1:2. Finally, azobisisobutyronitrile as an initiator is added, and its addition amount accounts for 2wt% of the total mass of 3-methacrylamide dopamine and methacrylic acid monomers to prepare an oil phase solution; a polyvinyl pyrrolidone aqueous solution with a mass concentration of 6wt% is used as an aqueous phase solution, and the oil phase solution is poured into the aqueous phase solution, and mechanically stirred at a speed of 1000r / min for emulsification for 10min; then, the temperature is raised to 70°C to carry out polymerization reaction under mechanical stirring for 6h, and the solution after the reaction is solid-liquid separated, and the obtained solid is washed and dried to obtain phase change microcapsules;

[0041] (3) The base fabric is immersed in a solution containing 20 wt% of phase change microcapsules, and allowed to stand for 1 hour to allow the phase change microcapsules to self-adhere to the base fabric. After being taken out, the solution is rolled and dried to obtain the temperature-regulating textile based on phase change microcapsules.

[0042] Sample analysis

[0043] The SEM images of the phase change microcapsules prepared by the methods in the representative examples 1 and 2 are shown as follows: Figure 1 and Figure 2 As shown, it can be seen that the morphology is regular and the particle size of the phase change microcapsules is small; the test shows that the encapsulation rate of the phase change microcapsules is 70-80%; the thermal enthalpy value of the phase change microcapsules prepared in Examples 1-3 is 125-170 J / g.

[0044] The performance of the temperature-regulating textiles based on phase change microcapsules prepared in Examples 1-3 was tested, and the basic fabric was used as a control. The basic fabric had no endothermic / exothermic peak and no heat storage function. The temperature-regulating textiles based on phase change microcapsules prepared in Examples 1-3 had excellent heat storage and temperature regulation functions, and their thermal enthalpy values ​​reached 80 to 98 J / g. The temperature-regulating textile in Example 1 had the highest thermal enthalpy value and the weight retention rate after washing reached more than 70%.

[0045] The embodiments described above provide a detailed description of the technical solutions of the present invention. It should be understood that the above are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, supplements or similar substitutions made within the scope of the principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing temperature-regulating textiles based on phase-change microcapsules, characterized in that: The following steps are involved: (1) using electrospinning to prepare nanofibers from a polymer solution, and then spinning and weaving the nanofibers with natural fibers to obtain a basic fabric; (2) After the paraffin is heated and melted, 3-methacrylamide dopamine and methacrylic acid are added, and finally an initiator is added to prepare an oil phase solution, and the oil phase solution is poured into an aqueous phase solution containing an emulsifier, stirred and emulsified, and heated to cause a polymerization reaction to obtain phase change microcapsules; (3) Soaking the base fabric in a solution containing phase change microcapsules to allow the phase change microcapsules to self-adhere to the base fabric, taking it out, rolling it, and drying it to obtain the temperature-regulating textile based on phase change microcapsules.

2. The method for preparing temperature-regulating textiles based on phase-change microcapsules according to claim 1, characterized in that: In step (1), the polymer includes polyvinyl alcohol, nylon, polylactic acid or polyurethane; the natural fiber is any one of cotton and linen.

3. The method for preparing temperature-regulating textiles based on phase-change microcapsules according to claim 1, characterized in that: In step (1), the concentration of the polymer solution is 13-20wt%; the parameters of the electrospinning process are: voltage 15-20kV, distance from spinneret to collector 15-20cm, flow rate 0.5-1.5mL / h, ambient temperature 20-30°C, and ambient humidity 40%-50%.

4. The method for preparing temperature-regulating textiles based on phase-change microcapsules according to claim 2, characterized in that: The mass ratio of nanofibers to natural fibers is 1:0.2-1.

5. The method for preparing temperature-regulating textiles based on phase-change microcapsules according to claim 1, characterized in that: Based on the total mass of two monomers, 3-methacrylamide dopamine and methacrylic acid, the mass ratio of paraffin to the two monomers is 1:0.1-1; the mass ratio of 3-methacrylamide dopamine to methacrylic acid is 1:1-2.

6. The method for preparing temperature-regulating textiles based on phase-change microcapsules according to claim 1, characterized in that: The mass concentration of the emulsifier in the aqueous phase solution is 1wt% to 8wt%, and the emulsifier is sodium dodecylbenzene sulfonate, polyvinyl pyrrolidone or polysorbate monoether.

7. The method for preparing temperature-regulating textiles based on phase-change microcapsules according to claim 1, characterized in that: The polymerization temperature is 60-90°C, and the polymerization reaction is carried out for 4-6 hours under mechanical stirring conditions.

8. The method for preparing temperature-regulating textiles based on phase-change microcapsules according to claim 1, characterized in that: In step (3), the mass concentration of the phase change microcapsules in the solution containing the phase change microcapsules is 10wt% to 20wt%, and the immersion time is 30min to 2h.

9. The temperature-regulating textile based on phase change microcapsules obtained according to the preparation method of the temperature-regulating textile based on phase change microcapsules according to any one of claims 1 to 8.

Citation Information

Patent Citations

  • Microcapsule finishing method for maintaining microenvironment of human body

    CN104250934A

  • Preparation method of paraffin phase-change microcapsule

    CN107722943A

  • Microcapsule phase-change temperature-adjusting lyocell fiber and preparation method thereof

    CN116121893A

  • Phase change microcapsule and preparation method thereof

    CN117821025A

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