阅读说明：本技术 调温纤维的制备方法、调温纤维和织物 (Preparation method of temperature-adjusting fiber, temperature-adjusting fiber and fabric ) 是由 马龙 林泽 于 2021-06-01 设计创作，主要内容包括：本申请涉及材料技术领域,具体而言,涉及一种调温纤维的制备方法、调温纤维和织物。调温纤维的制备方法包括以下步骤：制备核壳/相变材料复合颗粒；将第一组分和包含核壳/相变材料复合颗粒的第二组分通过喷丝板上的喷丝孔喷出,喷丝孔包括第一喷丝孔和被第一喷丝孔环绕的第二喷丝孔,第一组分从第一喷丝孔喷出,第二组分从第二喷丝孔喷出；从第一喷丝孔喷出的第一组分包裹从第二喷丝孔喷出的第二组分形成形成初生纤维,所述初生纤维先通过空气层,然后进入凝固浴,出浴后通过卷绕筒收集初生纤维,再在热水中拉伸获得调温纤维。相变材料温度低时可以放热变暖,从而起到温度调节作用,该相变材料位于纤维内部,可以耐摩擦洗涤。(The application relates to the technical field of materials, in particular to a temperature-adjusting fiber, a preparation method thereof and a fabric. The preparation method of the temperature-adjusting fiber comprises the following steps: preparing core-shell/phase-change material composite particles; spraying a first component and a second component containing core-shell/phase-change material composite particles through spinneret orifices on a spinneret plate, wherein the spinneret orifices comprise a first spinneret orifice and a second spinneret orifice surrounded by the first spinneret orifice, the first component is sprayed from the first spinneret orifice, and the second component is sprayed from the second spinneret orifice; and the first component sprayed from the first spinneret orifice wraps the second component sprayed from the second spinneret orifice to form nascent fiber, the nascent fiber firstly passes through an air layer and then enters a coagulating bath, the nascent fiber is collected through a winding drum after being taken out of the bath, and then the nascent fiber is stretched in hot water to obtain the temperature-adjusting fiber. The phase change material can release heat and warm when the temperature is low, so that the temperature adjusting effect is achieved, and the phase change material is located inside the fibers and can resist friction washing.)

1. The preparation method of the temperature-regulating fiber is characterized by comprising the following steps of:

step 1, preparing core-shell/phase-change material composite particles;

step 2, spraying a first component and a second component containing the core-shell/phase-change material composite particles through spinneret orifices on a spinneret plate, wherein the spinneret orifices comprise first spinneret orifices and second spinneret orifices surrounded by the first spinneret orifices, the first component is sprayed from the first spinneret orifices, and the second component is sprayed from the second spinneret orifices;

and 3, wrapping the second component sprayed from the second spinneret hole with the first component sprayed from the first spinneret hole to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fibers.

2. The method for preparing a temperature-regulating fiber according to claim 1, wherein the step 1 comprises:

step 101, uniformly mixing and dispersing a phase change material, a monomer for synthesizing a core shell, an initiator and a coupling agent to obtain a first mixed system;

102, adding an emulsifier into a solvent, and fully mixing to obtain a second mixed system;

103, uniformly mixing the first mixed system and the second mixed system to form an emulsion, and heating while stirring to initiate a polymerization reaction between monomers;

and step 104, washing and drying the reaction product after the reaction is finished to obtain the core-shell/phase-change material composite particles.

3. The method of claim 1, wherein the phase change material is selected from at least one of higher aliphatic hydrocarbons, fatty acids, alcohols, polyhydroxycarbonic acids, and polyolefins.

4. The method for preparing the temperature-regulating fiber according to claim 2, wherein the monomer is at least one of styrene, propylene, acrylonitrile, butadiene, methyl methacrylate and acrylic acid.

5. The method for preparing the temperature-regulating fiber according to claim 1, wherein the first component is a spinning solution, the second component is a powder composed of the core-shell/phase-change material composite particles, the first component is extruded out of the first spinneret hole through a spinning machine, and the second component is extruded out of the second spinneret hole through a powder gun.

6. The method of claim 1, wherein the first component is a spinning solution, the second component is a spinning solution containing the core-shell/phase-change material composite particles, the first component is extruded through the first spinneret hole by a spinning machine, and the second component is extruded through the second spinneret hole by the spinning machine.

7. The method for preparing the temperature-regulating fiber according to claim 5 or 6, wherein the spinning solution is a cellulose acetate spinning solution, a spandex spinning solution, a nylon spinning solution or a polyester spinning solution.

8. The method of claim 1, wherein the core-shell/phase change material composite particles have an average diameter of not greater than 8 μm, the first orifice has a diameter of 0.3 to 0.5mm, and the second orifice has a diameter of 0.1 to 0.25 mm.

9. A temperature control fiber prepared by the preparation method of any one of claims 1 to 8, wherein the temperature control fiber comprises an outer base layer and an inner phase change layer.

10. A fabric woven from the temperature-regulating fiber of claim 9.

Technical Field

The application relates to the technical field of materials, in particular to a preparation method of tree temperature-adjusting fibers, temperature-adjusting fibers and a fabric.

Background

At present, with the improvement of living standard of people, the requirements of consumers on the functionality and the comfort of textiles are higher and higher, wherein the demand of comfortable textiles is increasing. The regenerated cellulose fiber textile line adopts natural cellulose and/or cotton linter, and chemical fibers are obtained by spinning after spinning solution is prepared by a series of processing procedures, and textile products prepared by the chemical fibers have the characteristics of softness, moisture absorption and comfort.

In order to achieve a certain temperature regulation effect, the temperature regulation material is usually soaked in the surface of the fiber or is blended with the temperature regulation material, so that the clothing has a certain temperature regulation effect, can maintain proper temperature and enables a human body to feel comfortable. When the fabric is used, clothes need to be folded, unfolded, washed and the like frequently, the surface of the fiber or the blended temperature adjusting material can be damaged, and the temperature adjusting effect is reduced after the fabric is used for a certain time.

Disclosure of Invention

In order to solve the technical problems, namely how to solve the technical problem that the surface of the fiber is damaged or the blended temperature regulating material is damaged in the using process of clothes in the prior art, a preparation method of the temperature regulating fiber, the temperature regulating fiber and a fabric are provided.

In order to achieve the above object, according to a first aspect of the present invention, there is provided a method for producing a temperature-adjusting fiber.

The preparation method of the temperature-adjusting fiber comprises the following steps:

step 1, preparing core-shell/phase-change material composite particles;

step 2, spraying a first component and a second component containing the core-shell/phase-change material composite particles through spinneret orifices on a spinneret plate, wherein the spinneret orifices comprise first spinneret orifices and second spinneret orifices surrounded by the first spinneret orifices, the first component is sprayed from the first spinneret orifices, and the second component is sprayed from the second spinneret orifices;

and 3, wrapping the second component sprayed from the second spinneret hole by the first component sprayed from the first spinneret hole to form nascent fiber, allowing the nascent fiber to pass through an air layer and then enter a coagulating bath, collecting the nascent fiber through a winding drum after the nascent fiber is taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fiber.

Further, according to the preparation method of the temperature-adjusting fiber provided by the embodiment of the invention, the step 1 comprises the following steps:

step 101, uniformly mixing and dispersing a phase change material, a monomer for synthesizing a core shell, an initiator and a coupling agent to obtain a first mixed system;

102, adding an emulsifier into a solvent, and fully mixing to obtain a second mixed system;

103, uniformly mixing the first mixed system and the second mixed system to form an emulsion, and heating while stirring to initiate a polymerization reaction between monomers;

and step 104, washing and drying the reaction product after the reaction is finished to obtain the core-shell/phase-change material composite particles.

Further, according to the method for preparing the temperature control fiber provided by the embodiment of the invention, the phase change material is selected from at least one of higher aliphatic hydrocarbons, fatty acids, alcohols, polyhydroxy carbonic acids and polyolefins.

Further, according to the preparation method of the temperature-regulating fiber provided by the embodiment of the invention, the monomer is at least one of styrene, propylene, acrylonitrile, butadiene, methyl methacrylate and acrylic acid.

Further, according to the preparation method of the temperature-regulating fiber provided by the embodiment of the invention, the first component is spinning solution, the second component is powder composed of the core-shell/phase-change material composite particles, the first component is extruded out of the first spinneret hole through a spinning machine, and the second component is sprayed out of the second spinneret hole through a powder gun.

Further, according to the preparation method of the temperature-regulating fiber provided by the embodiment of the invention, the first component is a spinning solution, the second component contains a spinning solution of the core-shell/phase-change material composite particles, the first component is extruded out of the first spinneret hole through a spinning machine, and the second component is extruded out of the second spinneret hole through the spinning machine.

Further, according to the preparation method of the temperature-regulating fiber provided by the embodiment of the invention, the spinning solution is a cellulose acetate spinning solution, a spandex spinning solution, a nylon spinning solution or a polyester spinning solution.

Further, according to the preparation method of the temperature-regulating fiber provided by the embodiment of the invention, the average diameter of the core-shell/phase-change material composite particles is not more than 8 μm, the diameter of the first spinneret hole is 0.3-0.5mm, and the diameter of the second spinneret hole is 0.1-0.25 mm.

In order to achieve the above object, according to a second aspect of the present invention, there is also provided a temperature control fiber.

The temperature-regulating fiber according to the embodiment of the application is prepared by the preparation method of the temperature-regulating fiber provided by the first aspect of the application.

In order to achieve the above object, according to a third aspect of the present invention, there is also provided an aircloth.

According to the fabric of the embodiment, the fabric is woven by the temperature-adjusting fiber provided by the second aspect of the application.

The inside hollow pore that is formed with of the fibrous structure that adjusts the temperature that makes in this application, the pore intussuseption is filled with energy storage phase change material, and energy storage phase change material can absorb, store and release the heat, can absorb the heat cooling when the temperature is high, can release heat and warm when the temperature is low to play the temperature regulation effect, this phase change material is located inside the fibre, can rub-resistant washing.

Drawings

The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.

FIG. 1 is a cross-sectional view of a temperature control fiber according to an embodiment of the present invention;

fig. 2 is a schematic structural diagram of a spinneret plate used in the embodiment of the present invention.

Detailed Description

In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It should be understood that the data so used may be interchanged under appropriate circumstances such that embodiments of the application described herein may be used. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.

In this application, the terms "upper", "lower", "inner", "middle", "outer", "front", "rear", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings. These terms are used primarily to better describe the present application and its embodiments, and are not used to limit the indicated devices, elements or components to a particular orientation or to be constructed and operated in a particular orientation.

Moreover, some of the above terms may be used to indicate other meanings besides the orientation or positional relationship, for example, the term "on" may also be used to indicate some kind of attachment or connection relationship in some cases. The specific meaning of these terms in this application will be understood by those of ordinary skill in the art as appropriate.

Furthermore, the terms "disposed," "connected," and "secured" are to be construed broadly. For example, "connected" may be a fixed connection, a detachable connection, or a unitary construction; can be a mechanical connection, or an electrical connection; may be directly connected, or indirectly connected through intervening media, or may be in internal communication between two devices, elements or components. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.

It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.

The preparation method of the temperature-regulating fiber provided by the embodiment of the invention firstly prepares core-shell/phase-change material composite particles, then prepares spinning solution, and performs spinning through a spinneret plate with a special structure, so that the formed temperature-regulating fiber structure is shown in figure 1, the temperature-regulating fiber comprises a first part 1 and a second part 2 coated by the first part 1, wherein the first part 1 is formed by conventional spinning solution, and the second part 2 contains the core-shell/phase-change material composite particles.

In order to obtain the temperature-adjusting fiber shown in fig. 1, a spinneret plate structure shown in fig. 2 is designed, a first spinneret orifice 4 and a second spinneret orifice 5 are coaxially arranged on a spinneret plate 3, the first spinneret orifice 4 is sleeved outside the second spinneret orifice 5 and used for forming a first part 1 of the temperature-adjusting fiber, and the second spinneret orifice 5 is positioned inside the second part 2 of the temperature-adjusting fiber.

Of course, the cross-sectional shapes of the first spinneret orifice and the second spinneret orifice in the embodiment of the present invention are not limited to the circular shapes shown in the drawings of the present application, and may also be other special-shaped structures, including but not limited to T-shaped, Y-shaped, crescent, i-shaped, and the like, which may be specifically selected according to the needs, and the number of the spinneret orifices on the same spinneret plate is not specifically limited. For example, when cylindrical fibers are required, the jet hole structure shown in the drawing of the invention is preferably adopted, and the spinneret hole is circular, so that the proportion of fibers with circular cross sections can be maximized, the cross section shape of the fibers can be controlled, and the uniformity of the fiber structure can be guaranteed.

The diameter of the first spinneret orifice 4 is 0.3-0.5mm, the diameter of the second spinneret orifice 5 is 0.1-0.25mm, in order to enable the core-shell/phase-change material composite particles to smoothly pass through the second spinneret orifice 5 and keep good flowing smoothness, the maximum particle size of the core-shell/phase-change material composite particles is preferably not more than 25 micrometers, and the average diameter is not more than 8 micrometers. Preferably, the diameter of the first spinneret orifice 4 is 0.4mm, and the diameter of the second spinneret orifice 5 is 0.2mm, and the temperature-regulating fibers are prepared by using the spinneret orifices with the sizes in the examples and the comparative examples described below.

The second part of the temperature-adjusting fiber can be formed by uniformly mixing the core-shell/phase-change material composite particles with a conventional spinning solution and then extruding the core-shell/phase-change material composite particles through a spinning machine to form a second spinneret hole, or can be formed by directly spraying the core-shell/phase-change material composite particles out of the second spinneret hole through a powder spray gun, and the former is preferred because the diameter of the second spinneret hole is small, the mode of spraying dry powder by the powder spray gun is easy to cause blockage, and the realization difficulty is high.

The preparation of the core-shell/phase-change material composite particles in the embodiment of the invention can be realized by the following steps: uniformly mixing and dispersing a phase-change material, a monomer for synthesizing a core shell, an initiator and a coupling agent to obtain a first mixed system; adding an emulsifier into a solvent, and fully mixing to obtain a second mixed system; 103, uniformly mixing the first mixed system and the second mixed system to form an emulsion, and heating while stirring to initiate a polymerization reaction between monomers; and after the reaction is finished, washing and drying the reaction product to obtain the core-shell/phase-change material composite particles. Wherein the phase change material is selected from at least one of higher aliphatic hydrocarbons, fatty acids, alcohols, polyhydroxycarbonic acids, and polyolefins; the monomer is at least one of styrene, propylene, acrylonitrile, butadiene, methyl methacrylate and acrylic acid; the emulsifier is sodium dodecyl benzene sulfonate; the initiator includes but is not limited to azobisisobutyl; the coupling agent includes, but is not limited to, a silane coupling agent. Of course, the preparation of the core-shell/phase-change material composite particles in the embodiment of the invention can be realized by other methods, for example, the material of the core-shell can be selected from inorganic materials. It should be noted that, the second part of the temperature-adjusting fiber is formed by uniformly mixing the core-shell/phase-change material composite particles with a conventional spinning solution and extruding the mixture through a spinning machine to form a second spinneret hole, in the process, the solubility of the solvent and the core-shell is poor in the prepared spinning solution, so that the core-shell is prevented from being damaged by the spinning solution, and experiments show that when the spinning solution contains the solvent which enables the core-shell to be easily dissolved, the enthalpy value of the obtained temperature-adjusting fiber is reduced, and when the core-shell made of an inorganic material is adopted, the problem can be effectively overcome.

In the following, preferred embodiments of the present invention will be described in detail, and the diameter of the first spinneret hole 4 is 0.4mm and the diameter of the second spinneret hole 5 is 0.2mm in each example.

Example 1

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles:

stirring 73 parts by weight of capric acid, 22 parts by weight of styrene, 13 parts by weight of methyl methacrylate, 3 parts by weight of acrylic acid, 0.4 part by weight of silane coupling agent and 0.4 part by weight of azobisisobutyronitrile at 32 ℃ to uniformly disperse to obtain a first mixed system; stirring 3 parts by weight of sodium dodecyl sulfate and 450 parts by weight of deionized water at 30 ℃ to prepare a second mixed system; uniformly mixing the first mixed system and the second mixed system at the temperature of 30 ℃, stirring and emulsifying at the rotating speed of 6500r/min to prepare an emulsion, and heating the emulsion at 83 ℃ for 7 hours to perform polymerization reaction; and after the reaction is finished, washing and drying the reaction product to prepare the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles, wherein a washing medium used in the washing process is an ethanol water solution, and the mass ratio of ethanol to water is 1: 4.

And 2, taking the cellulose acetate spinning solution as a first component. Mixing and stirring 100 parts by weight of cellulose acetate spinning solution and 30 parts by weight of styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles for 5 hours to prepare a second component. After the first component and the second component are respectively metered by a metering pump, the first component is sprayed out from a first spinneret orifice, the second component is sprayed out from a second spinneret orifice, and the content of the microcapsule composite particles in a final product can be controlled by controlling the spinneret speed of the second component passing through the second spinneret orifice.

And 3, wrapping the second component sprayed from the second spinneret hole with the first component sprayed from the first spinneret hole to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fibers.

The styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles obtained in the example have a particle size distribution of 0.4-12 μm and a content of 28%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy of 55.7J/g, the phase-change temperature range of 30-34 ℃, and the enthalpy of the temperature-adjusting fiber is basically unchanged after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine.

Example 2

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles:

stirring and uniformly dispersing 85 parts by weight of capric acid, 20 parts by weight of styrene, 10 parts by weight of methyl methacrylate, 8 parts by weight of acrylic acid, 0.35 part by weight of silane coupling agent and 0.4 part by weight of azobisisobutyronitrile at 32 ℃ to obtain a first mixed system; stirring 3 parts by weight of sodium dodecyl sulfate and 400 parts by weight of deionized water at 30 ℃ to prepare a second mixed system; uniformly mixing the first mixed system and the second mixed system at the temperature of 30 ℃, stirring and emulsifying at the rotating speed of 6500r/min to prepare an emulsion, and heating the emulsion at 83 ℃ for 7 hours to perform polymerization reaction; and after the reaction is finished, washing and drying the reaction product to prepare the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles, wherein a washing medium used in the washing process is an ethanol water solution, and the mass ratio of ethanol to water is 1: 4.

And 2, taking the cellulose acetate spinning solution as a first component. Mixing and stirring 100 parts by weight of cellulose acetate spinning solution and 35 parts by weight of styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles for 5 hours to prepare a second component. After the first component and the second component are respectively metered by a metering pump, the first component is sprayed out from a first spinneret orifice, the second component is sprayed out from a second spinneret orifice, and the content of the microcapsule composite particles in a final product can be controlled by controlling the spinneret speed of the second component passing through the second spinneret orifice.

And 3, wrapping the second component sprayed from the second spinneret hole with the first component sprayed from the first spinneret hole to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fibers.

The particle size distribution of the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles obtained in the embodiment is 0.6-16 μm, and the content of the microcapsule composite particles in the temperature-adjusting fiber is 32%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy of 59.2J/g, the phase-change temperature range of 29-34 ℃, and the enthalpy of the temperature-adjusting fiber is basically unchanged after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine.

Example 3

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles:

uniformly stirring and dispersing 90 parts by weight of capric acid, 32 parts by weight of styrene, 15 parts by weight of methyl methacrylate, 5 parts by weight of acrylic acid, 0.5 part by weight of silane coupling agent and 0.5 part by weight of azobisisobutyronitrile at 32 ℃ to obtain a first mixed system; stirring 3.5 parts by weight of sodium dodecyl sulfate and 500 parts by weight of deionized water at 30 ℃ to prepare a second mixed system; uniformly mixing the first mixed system and the second mixed system at the temperature of 30 ℃, stirring and emulsifying at the rotating speed of 6500r/min to prepare an emulsion, and heating the emulsion at 83 ℃ for 7 hours to perform polymerization reaction; and after the reaction is finished, washing and drying the reaction product to prepare the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles, wherein a washing medium used in the washing process is an ethanol water solution, and the mass ratio of ethanol to water is 1: 4.

And 2, taking the cellulose acetate spinning solution as a first component. Mixing and stirring 100 parts by weight of cellulose acetate spinning solution and 20 parts by weight of styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles for 5 hours to prepare a second component. After the first component and the second component are respectively metered by a metering pump, the first component is sprayed out from a first spinneret orifice, the second component is sprayed out from a second spinneret orifice, and the content of the microcapsule composite particles in a final product can be controlled by controlling the spinneret speed of the second component passing through the second spinneret orifice.

And 3, wrapping the second component sprayed from the second spinneret hole with the first component sprayed from the first spinneret hole to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fibers.

The particle size distribution of the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles obtained in the embodiment is 0.5-15 μm, and the content of the microcapsule composite particles in the temperature-adjusting fiber is 22.5%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy value of 47.6J/g, the phase-change temperature range of 30-33 ℃, and the enthalpy value of the temperature-adjusting fiber is basically unchanged after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine.

Example 4

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing silicon dioxide/n-octadecane composite particles:

step 1, preparing silicon dioxide/n-octadecane composite particles:

stirring and uniformly dispersing 13 parts by weight of n-octadecane and 20 parts by weight of tetraethyl silicate at 36 ℃ to obtain a first mixed system; mixing 150 parts by weight of water, 125 parts by weight of ethanol and 5 parts by weight of cetrimide, and uniformly stirring at 36 ℃ to obtain a second mixed system; and (2) uniformly mixing the first mixed system and the second mixed system at the temperature of 36 ℃, stirring and emulsifying at the rotating speed of 2000r/min to prepare an emulsion, adding 4.8 parts by weight of 25 wt% ammonia water into the emulsion, keeping the temperature unchanged, and continuously stirring at the stirring speed of 600r/min for 10 hours, so that the tetraethyl silicate is subjected to hydrolysis reaction. And after the reaction is finished, washing and drying the reaction product to prepare the silicon dioxide/n-octadecane composite particles, wherein the washing medium used in the washing process is deionized water, and the drying temperature is 45 ℃.

And 2, taking the spandex spinning solution as a first component, mixing 100 parts by weight of the spandex spinning solution and 25 parts by weight of the silicon dioxide/n-octadecane composite particles, and stirring for 5 hours to obtain a second component. After the first component and the second component are respectively metered by a metering pump, the first component is sprayed out from a first spinneret orifice, the second component is sprayed out from a second spinneret orifice, and the content of the microcapsule composite particles in a final product can be controlled by controlling the spinneret speed of the second component passing through the second spinneret orifice.

And 3, wrapping the second component sprayed from the second spinneret hole with the first component sprayed from the first spinneret hole to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fibers.

The particle size distribution of the silica/n-octadecane composite particles obtained in the example is 0.3-3 μm, and the content of the microcapsule composite particles in the temperature-adjusting fiber is 30.4%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy of 76.9J/g, the phase-change temperature range of 28-29.5 ℃, and the enthalpy of the temperature-adjusting fiber is basically unchanged after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine.

Example 5

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles:

uniformly stirring and dispersing 77 parts by weight of capric acid, 35 parts by weight of styrene, 10 parts by weight of methyl methacrylate, 10 parts by weight of acrylic acid, 0.5 part by weight of silane coupling agent and 0.5 part by weight of azobisisobutyronitrile at 32 ℃ to obtain a first mixed system; stirring 3 parts by weight of sodium dodecyl sulfate and 550 parts by weight of deionized water at 30 ℃ to prepare a second mixed system; uniformly mixing the first mixed system and the second mixed system at the temperature of 30 ℃, stirring and emulsifying at the rotating speed of 6500r/min to prepare an emulsion, and heating the emulsion at 83 ℃ for 7 hours to perform polymerization reaction; and after the reaction is finished, washing and drying the reaction product to prepare the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles, wherein a washing medium used in the washing process is an ethanol water solution, and the mass ratio of ethanol to water is 1: 4.

Step 2, using the polyamide spinning solution as a first component; mixing and stirring 100 parts by weight of nylon spinning solution and 20 parts by weight of styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles for 5 hours to prepare a second component. After the first component and the second component are respectively metered by a metering pump, the first component is sprayed out from a first spinneret orifice, the second component is sprayed out from a second spinneret orifice, and the content of the microcapsule composite particles in a final product can be controlled by controlling the spinneret speed of the second component passing through the second spinneret orifice.

And 3, wrapping the second component sprayed from the second spinneret hole with the first component sprayed from the first spinneret hole to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fibers.

The particle size grade of the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles obtained in the example is 0.5-14 μm, and the content of the microcapsule composite particles in the temperature-adjusting fiber is 21.7%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy value of 45.5J/g, the phase-change temperature range of 30-33 ℃, and the enthalpy value of the temperature-adjusting fiber is basically unchanged after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine.

Example 6

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles:

stirring and uniformly dispersing 100 parts by weight of capric acid, 25 parts by weight of styrene, 20 parts by weight of methyl methacrylate, 8 parts by weight of acrylic acid, 0.5 part by weight of silane coupling agent and 0.5 part by weight of azobisisobutyronitrile at 32 ℃ to obtain a first mixed system; stirring 4.5 parts by weight of sodium dodecyl sulfate and 500 parts by weight of deionized water at 30 ℃ to prepare a second mixed system; uniformly mixing the first mixed system and the second mixed system at the temperature of 30 ℃, stirring and emulsifying at the rotating speed of 6500r/min to prepare an emulsion, and heating the emulsion at 83 ℃ for 7 hours to perform polymerization reaction; and after the reaction is finished, washing and drying the reaction product to prepare the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles, wherein a washing medium used in the washing process is an ethanol water solution, and the mass ratio of ethanol to water is 1: 4.

And 2, taking the polyester spinning solution as a first component. Mixing and stirring 100 parts by weight of polyester spinning solution and 30 parts by weight of styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles for 5 hours to prepare a second component. After the first component and the second component are respectively metered by a metering pump, the first component is sprayed out from a first spinneret orifice, the second component is sprayed out from a second spinneret orifice, and the content of the microcapsule composite particles in a final product can be controlled by controlling the spinneret speed of the second component passing through the second spinneret orifice.

And 3, wrapping the second component sprayed from the second spinneret hole with the first component sprayed from the first spinneret hole to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fibers.

The particle size distribution of the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles obtained in the embodiment is 0.6-17.5 μm, and the content of the microcapsule composite particles in the temperature-adjusting fiber is 23.2%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy of 57.9J/g, the phase-change temperature range of 30-33 ℃, and the enthalpy of the temperature-adjusting fiber is basically unchanged after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine.

Example 7

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing silicon dioxide/n-octadecane composite particles:

stirring and uniformly dispersing 15 parts by weight of n-octadecane and 23 parts by weight of tetraethyl silicate at 36 ℃ to obtain a first mixed system; mixing 180 parts by weight of water, 140 parts by weight of ethanol and 5.6 parts by weight of cetrimide, and uniformly stirring at 36 ℃ to obtain a second mixed system; and uniformly mixing the first mixed system and the second mixed system at the temperature of 36 ℃, stirring and emulsifying at the rotating speed of 2000r/min to prepare an emulsion, adding 5.5 parts by weight of 25 wt% ammonia water into the emulsion, keeping the temperature unchanged, and continuously stirring for 10 hours at the stirring speed of 600r/min, so that the tetraethyl silicate is subjected to hydrolysis reaction. And after the reaction is finished, washing and drying the reaction product to prepare the silicon dioxide/n-octadecane composite particles, wherein the washing medium used in the washing process is deionized water, and the drying temperature is 45 ℃.

Step 2, using the polyamide spinning solution as a first component; mixing and stirring 100 parts by weight of nylon spinning solution and 20 parts by weight of silicon dioxide/n-octadecane composite particles for 4.5 hours to prepare a second component. After the first component and the second component are respectively metered by a metering pump, the first component is sprayed out from a first spinneret orifice, the second component is sprayed out from a second spinneret orifice, and the content of the microcapsule composite particles in a final product can be controlled by controlling the spinneret speed of the second component passing through the second spinneret orifice.

And 3, wrapping the second component sprayed from the second spinneret hole with the first component sprayed from the first spinneret hole to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching in hot water to obtain the temperature-adjusting fibers.

The particle size grade of the silica/n-octadecane composite particles obtained in the example is 0.35-4 μm, and the content of the microcapsule composite particles in the temperature-adjusting fiber is 28.4%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy value of 72.4J/g, the phase-change temperature range of 28-30.5 ℃, and the enthalpy value of the temperature-adjusting fiber is basically unchanged after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine.

Comparative example 1

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles:

stirring 73 parts by weight of capric acid, 22 parts by weight of styrene, 13 parts by weight of methyl methacrylate, 3 parts by weight of acrylic acid, 0.4 part by weight of silane coupling agent and 0.4 part by weight of azobisisobutyronitrile at 32 ℃ to uniformly disperse to obtain a first mixed system; stirring 3 parts by weight of sodium dodecyl sulfate and 450 parts by weight of deionized water at 30 ℃ to prepare a second mixed system; uniformly mixing the first mixed system and the second mixed system at the temperature of 30 ℃, stirring and emulsifying at the rotating speed of 6500r/min to prepare an emulsion, and heating the emulsion at 83 ℃ for 7 hours to perform polymerization reaction; and after the reaction is finished, washing and drying the reaction product to prepare the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles, wherein a washing medium used in the washing process is an ethanol water solution, and the mass ratio of ethanol to water is 1: 4.

And 2, mixing 100 parts by weight of cellulose acetate spinning solution and 14 parts by weight of styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles, and stirring for 4 hours to form a mixed system. Metering the mixed system by a metering pump, spraying out the mixed system through a spinneret orifice on a conventional spinneret plate to form nascent fiber, allowing the nascent fiber to pass through an air layer and then enter a coagulating bath, collecting the nascent fiber through a winding drum after the nascent fiber is taken out of the bath, and stretching the nascent fiber in hot water to obtain the temperature-regulating fiber.

The content of the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles in the temperature-adjusting fiber obtained in this example was 28%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy of 56.1J/g, the phase-change temperature range of 30-34 ℃, and the enthalpy of the temperature-adjusting fiber is reduced by 13% after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine. It can be seen that in the case of the temperature-adjusting fiber without a coating layer on the outer surface, the water washing can cause the loss of the microcapsule particles, mainly because the diameter of the temperature-adjusting fiber is in the micron order, and the temperature-adjusting fiber has a large specific surface area, although the microcapsule particles are mixed with the spinning solution, a considerable proportion of the microcapsule particles are still located behind the surface of the fiber and close to the surface of the fiber, and the microcapsule particles are easy to separate after being disturbed to some extent.

Comparative example 2

A method of making a temperature regulating fiber comprising the steps of:

step 1, preparing styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particle emulsion.

Stirring 73 parts by weight of capric acid, 22 parts by weight of styrene, 13 parts by weight of methyl methacrylate, 3 parts by weight of acrylic acid, 0.4 part by weight of silane coupling agent and 0.4 part by weight of azobisisobutyronitrile at 32 ℃ to uniformly disperse to obtain a first mixed system; stirring 3 parts by weight of sodium dodecyl sulfate and 450 parts by weight of deionized water at 30 ℃ to prepare a second mixed system; and (2) uniformly mixing the first mixed system and the second mixed system at the temperature of 30 ℃, stirring and emulsifying at the rotating speed of 6500r/min to prepare an emulsion, and heating the emulsion at 83 ℃ for 7 hours to perform polymerization reaction.

And 2, metering the cellulose acetate spinning solution by a metering pump, spraying the cellulose acetate spinning solution through a spinneret orifice on a conventional spinneret plate to form nascent fibers, allowing the nascent fibers to pass through an air layer and then enter a coagulating bath, collecting the nascent fibers through a winding drum after the nascent fibers are taken out of the bath, and stretching the nascent fibers in hot water to obtain the cellulose acetate fibers.

And 3, immersing the acetate fiber obtained in the step 2 into the emulsion system after the reaction in the step 1 at the temperature of 75 ℃, padding the acetate fiber for 20min, and drying at the temperature of 80 ℃ to obtain the temperature-adjusting fiber.

The content of the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles in the temperature-adjusting fiber obtained in this example was 24%. Tests prove that the temperature-adjusting fiber prepared by the embodiment has the enthalpy of 49.1J/g, the phase-change temperature range of 30-35 ℃, and the enthalpy of the temperature-adjusting fiber is reduced by 72% after the temperature-adjusting fiber is continuously washed for 120 hours by a washing machine.

In the process of implementing the method for preparing the temperature-regulating fiber of the present invention, when the phase-change material used is styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles, the second spinneret holes are often blocked, for example, in example 1, the second spinneret holes are blocked after 4.6 hours of continuous operation. When the styrene-methyl methacrylate-acrylic acid copolymer/capric acid composite particles are classified by screening, only the composite particles with the particle size of below 2.5 microns are selected to participate in forming the second component, and other process conditions are kept the same as those in example 1, the second spinning hole is basically free from blockage accidents, and continuous production can be realized, but the mode can cause serious waste of the composite particles. The technical personnel further study and find that the fluidity of the second component material can be optimized by adjusting the proportion range between the coarse and fine particle fractions of the composite particles, when the content of the particle fraction below 2.5 mu m is 15% -30%, the content of the particle fraction above 2.5 mu m-8.0 mu m is 50% -65% and the content of the particle fraction above 8.0 mu m is 5% -20%, other process conditions are kept the same as those in example 1, and at this time, the second spinning holes basically do not have blockage accidents, and the continuous production can be realized. The classification method for the composite particles can adopt a high-speed centrifugal classification method, a filter membrane classification method or an air sedimentation method, and the data are obtained based on the high-speed centrifugal classification method.

Some embodiments in this specification are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.

The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.