阅读说明：本技术 胶囊、含胶囊的织物及其制备方法和应用 (Capsule, fabric containing capsule, preparation method and application thereof ) 是由 鲍刘兵 刘宏伟 陈蕾 于 2020-12-01 设计创作，主要内容包括：本发明公开了胶囊、含胶囊的织物及其制备方法和应用,涉及纺织面料功能性整理技术领域,包括以下重量比的原料：胶囊35～50份,导热填料0～20份,交联剂3～10份,增稠剂1～4份,渗透剂0.1～1份,消泡剂0.1～0.5份,纯水,胶囊表面的-OH、-NH-2等极性基团与植物纤维表面的活性基团形成较强的相互作用,添加少量交联剂即可进一步提高耐洗涤效果并保证制备的各种材质调温织物耐洗涤牢度,低交联剂使用量有利于改善织物手感,提高织物透气性,由于壳聚糖季铵盐自身具有抗菌性,采用其改性的胶囊使得制备的相变调温织物同时具有一定抗菌功能。(The invention discloses a capsule, a fabric containing the capsule, a preparation method and an application thereof, relating to the technical field of functional finishing of textile fabrics, and the capsule comprises the following raw materials in percentage by weight: 35-50 parts of capsules, 0-20 parts of heat-conducting filler, 3-10 parts of cross-linking agent, 1-4 parts of thickening agent, 0.1-1 part of penetrating agent, 0.1-0.5 part of defoaming agent, pure water, and-OH and-NH on the surfaces of the capsules 2 The polar groups and the active groups on the surface of the plant fiber form stronger interaction, a small amount of cross-linking agent is added to further improve the washing fastness and ensure the washing fastness of the prepared temperature-regulating fabric made of various materials, the use amount of the cross-linking agent is low, the hand feeling of the fabric is improved, the air permeability of the fabric is improved, and the phase-change temperature-regulating fabric prepared by adopting the modified capsule has a certain antibacterial function due to the antibacterial property of the chitosan quaternary ammonium salt.)

1. The capsule is characterized by comprising a phase-change microcapsule and chitosan quaternary ammonium salt coated on the surface of the phase-change microcapsule, wherein the weight ratio of the chitosan quaternary ammonium salt to the phase-change microcapsule is as follows: 1-3: 1;

the particle size of the phase change microcapsule is 0.1-100 mu m;

the substitution degree of the chitosan quaternary ammonium salt is more than 90.0 percent.

2. A method of making the capsule of claim 1, comprising the steps of:

(1) dissolving chitosan quaternary ammonium salt in water, and dissolving the chitosan quaternary ammonium salt in pure water at 50-70 ℃ under the stirring of 80-120 rpm to prepare a chitosan quaternary ammonium salt solution with the mass fraction of 6-10%;

(2) slowly adding the chitosan quaternary ammonium salt solution prepared in the step (1) into pre-dispersed aqueous phase-change microcapsule slurry, stirring at 600-1000 rpm for 20-50 min, and then adding a defoaming agent for defoaming, wherein the non-volatile matter content of the phase-change microcapsule slurry is 30-50%;

(3) uniformly coating chitosan quaternary ammonium salt on the surface of the phase change microcapsule by the mixed solution prepared in the step (2) through a spray drying process, wherein the spray drying condition is as follows: and collecting the powder to obtain the surface modified capsule, wherein the air inlet temperature is 165-195 ℃, the air outlet temperature is 80-100 ℃, and the air pressure is 0.1-0.5 MPa.

3. A capsule-containing fabric is characterized by comprising the following raw materials in percentage by weight:

35-50 parts of capsules, 0-20 parts of heat-conducting filler, 3-10 parts of cross-linking agent, 1-4 parts of thickening agent, 0.1-1 part of penetrating agent, 0.1-0.5 part of defoaming agent and pure water;

the capsule according to claim 1 or 2.

4. The capsule-containing fabric of claim 3, wherein the thermally conductive filler is one or a mixture of boron nitride, aluminum oxide, magnesium oxide, aluminum hydroxide, graphite and graphene.

5. The capsule-containing fabric of claim 3, wherein the cross-linking agent is one or a mixture of polyfunctional aziridine, sodium tripolyphosphate, epichlorohydrin, genipin, glutaraldehyde, and isocyanate.

6. The encapsulated fabric of claim 3 wherein said thickener is one or a mixture of cellulosics, polyacrylics, or polyurethanes.

7. The capsule-containing fabric of claim 3, wherein the osmotic agent is one or a mixture of fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene ether, sec-octanol polyoxyethylene ether and isooctanol polyoxyethylene ether.

8. The capsule-containing fabric of claim 3, wherein the antifoaming agent is a silicone-based antifoaming agent or a mineral oil-based antifoaming agent.

9. A method of making the capsule-containing fabric of any one of claims 3 to 8, comprising:

(1) mixing the chitosan quaternary ammonium salt surface-modified capsule powder, a heat-conducting filler, a cross-linking agent, a thickening agent, a penetrating agent, a defoaming agent and pure water according to the weight ratio, stirring for 10-20 min until the viscosity is more than 8000cps, and discharging;

(2) preparing the capsule finishing slurry prepared in the step (1) into a temperature-adjusting fabric through a rotary screen printing process, drying, and carrying out curing and crosslinking;

(3) and (3) washing the fabric prepared in the step (2), and finally carrying out heat setting treatment to obtain the fabric containing the surface modified phase change microcapsules.

10. Use of the capsule-containing fabric of claim 9 in the preparation of textile products including clothing, gloves, scarves, bed sheets, comforters, towels, socks, medical accessories and health care products.

Technical Field

The invention relates to the technical field of functional finishing of textile fabrics, in particular to capsules, a fabric containing the capsules, and a preparation method and application thereof.

Background

The phase change microcapsule comprises an organic polymer or inorganic wall material and a phase change core material coated by the organic polymer or inorganic wall material, is applied to the functional finishing research of fabrics, and has been used for years. The phase-change microcapsule can be well used for preparing temperature-adjusting fabrics by a finishing process based on the fact that the phase-change core material is subjected to solid-liquid reversible phase change after being heated in a cooling mode, so that the release and storage of heat energy are easy to realize.

Microcapsules act on fabrics primarily in two ways, one is the direct spinning process (incorporating microcapsules into the fibers) and one is the post-finishing process. The spinning method has severe requirements on the process technology and various properties of materials, and the post-finishing method mainly comprises dipping, padding, coating and the like, wherein the coating method is easy to implement, can endow the fabric with new functional characteristics under the condition of keeping the original mechanical strength of the fiber, and is often adopted in practical application. The coating method mechanically bonds the functional material to the surface of the fabric through the adhesive or the cross-linking agent, the method has higher requirements on the performance and the dosage of the adhesive, the phase-change microcapsules are easy to fall off when the dosage of the adhesive is less, the fabric air permeability and the hand feeling are poor when the dosage is high, and chemical groups capable of directly reacting are lacked between the microcapsules and the adhesive and between the microcapsules and the fabric fibers under most conditions, and the microcapsules are easy to fall off from the fabric along with the increase of washing times to lose the temperature regulation performance. At present, the fabrics which are subjected to functional finishing by adopting a mode of combining an adhesive and fibers have washing resistance times (the function is not lower than 50-80% after finishing) of 5-15 times, which greatly limits the long-term exertion of a certain function endowed by the specially-finished fabrics.

Disclosure of Invention

1. Technical problem to be solved by the invention

Aiming at the technical problem that the microcapsules are easy to fall off from the fabric along with the increase of the washing times and lose the temperature regulation performance, the invention provides the capsules, the fabric containing the capsules, and a preparation method and application thereof.

2. Technical scheme

In order to solve the problems, the technical scheme provided by the invention is as follows: a capsule comprises a phase change microcapsule and chitosan quaternary ammonium salt coated on the surface of the phase change microcapsule, wherein the weight ratio of the chitosan quaternary ammonium salt to the phase change microcapsule is as follows: 1-3: 1; the particle size of the phase change microcapsule is 0.1-100 mu m; the substitution degree of the chitosan quaternary ammonium salt is more than 90.0 percent. The phase-change microcapsule wall material is one or more composite film materials of polystyrene, polyurea, polyurethane, polyvinyl chloride, melamine resin, polyacrylate, polymethacrylate, polyvinyl alcohol and silicon dioxide; the phase-change microcapsule core material is paraffin.

The invention also discloses a method for preparing the capsule, which comprises the following steps:

(1) dissolving chitosan quaternary ammonium salt in water, and dissolving the chitosan quaternary ammonium salt in pure water at 50-70 ℃ under the stirring of 80-120 rpm to prepare a chitosan quaternary ammonium salt solution with the mass fraction of 6-10%;

(2) slowly adding the chitosan quaternary ammonium salt solution prepared in the step (1) into pre-dispersed aqueous phase-change microcapsule slurry, stirring at 600-1000 rpm for 20-50 min, and then adding a defoaming agent for defoaming, wherein the non-volatile matter of the phase-change microcapsule slurry is 30-50%, the aqueous phase-change microcapsule slurry is aqueous phase dispersion slurry of phase-change microcapsules, the aqueous phase-change microcapsule slurry is produced by the company, belongs to a finished product, does not need to be prepared additionally, and the solid content of the aqueous phase-change microcapsule slurry is 38%;

(3) uniformly coating chitosan quaternary ammonium salt on the surface of the phase change microcapsule by the mixed solution prepared in the step (2) through a spray drying process, wherein the spray drying condition is as follows: and collecting the powder to obtain the surface modified capsule, wherein the air inlet temperature is 165-195 ℃, the air outlet temperature is 80-100 ℃, and the air pressure is 0.1-0.5 MPa.

The invention also discloses capsule finishing size containing the capsule fabric, which comprises the following raw materials in percentage by weight:

35-50 parts of capsules, 0-20 parts of heat-conducting filler, 3-10 parts of cross-linking agent, 1-4 parts of thickening agent, 0.1-1 part of penetrating agent, 0.1-0.5 part of defoaming agent and pure water; the capsule is as described above.

Optionally, the heat conducting filler is one or a mixture of several of boron nitride, aluminum oxide, magnesium oxide, aluminum hydroxide, graphite and graphene.

Optionally, the cross-linking agent is one or a mixture of several of polyfunctional aziridine, sodium tripolyphosphate, epichlorohydrin, genipin, glutaraldehyde and isocyanate.

Optionally, the thickener is one or a mixture of more of celluloses, polyacrylics or polyurethanes.

Optionally, the penetrating agent is one or a mixture of several of fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene ether, sec-octanol polyoxyethylene ether and isooctanol polyoxyethylene ether.

Optionally, the defoaming agent is an organic silicon defoaming agent or a mineral oil defoaming agent.

The present invention also discloses a method of preparing a fabric containing capsules as described above, comprising:

(1) mixing the chitosan quaternary ammonium salt surface-modified capsule powder, a cross-linking agent, a thickening agent, a penetrating agent, a defoaming agent and pure water according to the weight ratio, stirring for 10-20 min until the viscosity is more than 8000cps, and discharging;

(2) preparing the capsule finishing slurry prepared in the step (1) into a temperature-adjusting fabric through a rotary screen printing process, drying, and carrying out curing and crosslinking;

(3) and (3) washing the fabric prepared in the step (2), and finally carrying out heat setting treatment to obtain the fabric containing the surface modified capsules.

The invention also discloses application of the fabric containing the capsules in preparation of textile products, wherein the textile products comprise clothes, gloves, scarves, bedsheets, quilt covers, towels, socks, medical accessories and health-care products.

3. Advantageous effects

Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:

(1) the capsule provided by the embodiment of the application adopts chitosan quaternary ammonium salt to physically coat the surface of the phase change microcapsule, so as to introduce-OH and-NH₂The reactive groups increase the surface adhesiveness of the phase change microcapsule, the surface coating treatment also improves the compactness of the wall material of the phase change microcapsule, thereby reducing the risk of leakage of the phase change material in the later use process, and the surface modification method of the phase change microcapsule adopts a physical spray drying method, does not limit the application of specific groups on the surface of the phase change microcapsule, and has potential wide applicability.

(2) The textile containing capsules provided by the embodiment of the application has modified-OH and-NH on the surfaces of the capsules₂Isopolar group and plant fiberActive groups on the surface of the fiber form stronger interaction, the washing fastness of the prepared temperature-regulating fabric made of various materials can be further improved by adding a small amount of cross-linking agent, the hand feeling of the fabric can be improved by using low dosage of the cross-linking agent, the air permeability of the fabric can be improved, and the phase-change temperature-regulating fabric prepared by adopting the modified capsule has a certain antibacterial function because the chitosan quaternary ammonium salt has antibacterial property.

Drawings

FIG. 1 is an optical microscope image of a 20-wash capsule-containing fabric prepared according to example 1 of the present invention.

Detailed Description

For a further understanding of the present invention, reference will now be made in detail to the embodiments illustrated in the drawings.

The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings. The terms first, second, and the like in the present invention are provided for convenience of describing the technical solution of the present invention, and have no specific limiting effect, but are all generic terms, and do not limit the technical solution of the present invention. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. Unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are intended to be inclusive and mean, for example, that they may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art. The technical solutions in the same embodiment and the technical solutions in different embodiments can be arranged and combined to form a new technical solution without contradiction or conflict, and the technical solutions are within the scope of the present invention.

Example 1

a. Preparation of capsules

(1) And dissolving the chitosan quaternary ammonium salt in pure water at 50-70 ℃ under stirring at 80-120 rpm to prepare a chitosan quaternary ammonium salt solution with the mass fraction of 6-10%. When the reaction temperature is lower than 50 ℃, the stirring speed is lower than 80rpm, the solubility of the quaternary ammonium salt of chitosan in water is poor, when the reaction temperature is higher than 70 ℃, the stirring speed is higher than 120rpm, the chemical property of the quaternary ammonium salt of chitosan is unstable and easy to decompose, when the mass fraction of the prepared quaternary ammonium salt solution of chitosan is lower than 6%, the coating rate of the quaternary ammonium salt of chitosan on the surface of the phase-change microcapsule is low, the modification effect is influenced, and when the mass fraction of the prepared quaternary ammonium salt solution of chitosan is higher than 10%, the waste of the quaternary ammonium salt of chitosan is easily caused;

(2) slowly adding the chitosan quaternary ammonium salt solution prepared in the step (1) into pre-dispersed aqueous phase-change microcapsule slurry, stirring at 600-1000 rpm for 20-50 min, and then adding a defoaming agent for defoaming, wherein the non-volatile matter content of the phase-change microcapsule slurry is 30-50%; when the stirring speed is lower than 600rpm, the stirring time is lower than 20min, the coating rate of the chitosan quaternary ammonium salt on the surface of the phase-change microcapsule is low, the modification effect is influenced, when the stirring speed is higher than 1000rpm, the stirring time is higher than 50min, the chitosan quaternary ammonium salt can fall off from the surface of the phase-change microcapsule, when the non-volatile content of the phase-change microcapsule slurry is lower than 30%, the coating rate of the chitosan quaternary ammonium salt on the surface of the phase-change microcapsule is low, the modification effect is influenced, and when the non-volatile content of the phase-change microcapsule slurry is higher than 50%, the cost is;

(3) uniformly coating chitosan quaternary ammonium salt on the surface of the phase change microcapsule by the mixed solution prepared in the step (2) through a spray drying process, wherein the spray drying condition is as follows: the air inlet temperature is 165-195 ℃, the air outlet temperature is 80-100 ℃, and the air pressure is 0.1-0.5 MPa, and the surface modified capsule is obtained by collecting powder. When the air inlet temperature is lower than 165 ℃, the air outlet temperature is lower than 80 ℃, the air pressure is lower than 0.1MPa, the capsule dryness is not enough, and when the air inlet temperature is higher than 195 ℃, the air outlet temperature is higher than 100 ℃, and the air pressure is higher than 0.9MPa, the chemical property of the capsule is easy to be unstable and the capsule is decomposed.

In this embodiment, the chitosan quaternary ammonium salt is dissolved in pure water at 60 ℃ under stirring at 100rpm to prepare a chitosan quaternary ammonium salt solution with a mass fraction of 8%, and then the chitosan quaternary ammonium salt solution is slowly added into the pre-dispersed aqueous phase change microcapsule slurry, wherein the amount of the chitosan quaternary ammonium salt is calculated according to the weight ratio of the chitosan quaternary ammonium salt to the phase change microcapsule, that is, the chitosan quaternary ammonium salt: the phase change microcapsule is 1:1, the nonvolatile content of the microcapsule slurry is 40%, stirring is carried out for 30min at 800rpm, mineral oil defoaming agents are added for defoaming, and then chitosan quaternary ammonium salt is uniformly coated on the surface of the phase change microcapsule by a spray drying process, wherein the spray drying conditions are as follows: the inlet air temperature is 175 ℃; the air outlet temperature is 90 ℃; the air pressure is 0.2 MPa; the obtained powder is the surface modified capsule. The surface of the phase change microcapsule is physically coated by chitosan quaternary ammonium salt, so that-OH and-NH are introduced₂The reactive groups increase the surface adhesiveness of the phase change microcapsule, the surface coating treatment also improves the compactness of the wall material of the phase change microcapsule, thereby reducing the risk of leakage of the phase change material in the later use process, and the surface modification method of the phase change microcapsule adopts a physical spray drying method, does not limit the application of specific groups on the surface of the phase change microcapsule, and has potential wide applicability.

In other embodiments, the reaction temperature in step (1) may be 50 ℃, 55 ℃, 65 ℃, 70 ℃, the stirring rate may be 80rpm, 90rpm, 110rpm, 120rpm, and the mass fraction of the chitosan quaternary ammonium salt solution may be 6%, 7%, 9%, 10%.

The stirring speed in the step (2) can be 600rpm, 700rpm, 900rpm and 1000rpm, the reaction time can be 20min, 25min, 40min and 50min, and the non-volatile content of the phase-change microcapsule slurry can be 30%, 35%, 45% and 50%.

The air inlet temperature in step (3) can be 165 deg.C, 170 deg.C, 180 deg.C, 195 deg.C, the air outlet temperature can be 80 deg.C, 85 deg.C, 95 deg.C, 100 deg.C, and the air pressure can be 0.1MPa, 0.3MPa, 0.4MPa, 0.15 MPa.

b. Preparation of Capsule-containing Fabric

(1) Mixing 35-50 parts by weight of surface-modified capsules, 0-20 parts by weight of heat conducting filler, 3-10 parts by weight of cross-linking agent, 1-4 parts by weight of thickening agent, 0.1-1 part by weight of penetrating agent, 0.1-0.5 part by weight of defoaming agent and pure water, stirring for 10-20 min until the viscosity is more than 8000cps, and discharging;

(2) preparing the capsule finishing slurry prepared in the step (1) into a temperature-adjusting fabric through a rotary screen printing process, drying, and carrying out curing and crosslinking;

(3) and (3) washing the fabric prepared in the step (2), and finally carrying out heat setting treatment to obtain the fabric containing the surface modified phase change microcapsules.

In this example, 50 parts of surface-modified capsule powder, 6 parts of aziridine crosslinking agent, 3 parts of sodium polyacrylate thickener, 0.1 part of JFC penetrant, 0.1 part of silicone defoamer and 40.8 parts of pure water were mixed, stirred at 1000rpm for 10min until the viscosity became more than 8000cps, and discharged; then preparing the prepared capsule finishing slurry into a temperature-adjusting fabric by a rotary screen printing process, wherein the fabric is all-cotton poplin, a machine roller magnetic rod No. 16, the speed of the machine is 20 yards, the drying temperature is 135 ℃, the printed coating is kept in a hot air oven for about 2min, and finally, the temperature-adjusting fabric is sequentially subjected to water washing and 180 ℃ heat setting treatment; thus obtaining the capsule-containing fabric of the invention. modified-OH, -NH of capsule surface₂The isopolar groups and active groups on the surface of the plant fiber form stronger interaction, a small amount of cross-linking agent is added to further improve the washing resistance effect and ensure the washing fastness of the prepared temperature-regulating fabric made of various materials, the use amount of the cross-linking agent is low, the hand feeling of the fabric is improved, the air permeability of the fabric is improved, and the chitosan quaternary ammonium salt has antibacterial property and is adopted to modify the capsule so that the modified capsule can ensure that the fabric has stronger washing resistance effectThe prepared phase-change temperature-regulating fabric has a certain antibacterial function.

In other embodiments, the capsule powder can be 35 parts, 40 parts and 45 parts, the heat conducting filler can be 5 parts, 10 parts, 15 parts and 20 parts, the cross-linking agent can be 3 parts, 5 parts, 7 parts and 10 parts, the penetrating agent can be 0.3 part, 0.5 part, 0.7 part and 1.0 part, the defoaming agent can be 0.2 part, 0.3 part, 0.4 part and 0.5 part, and the stirring time can be 12min, 14min, 16min, 18min and 20 min.

Example 2

a. Preparation of capsules

Firstly, dissolving chitosan quaternary ammonium salt in pure water at 60 ℃ under stirring at 100rpm to prepare a chitosan quaternary ammonium salt solution with the mass fraction of 8%; slowly adding the chitosan quaternary ammonium salt solution into the phase-change microcapsule slurry which is dispersed in advance, wherein the dosage of the chitosan quaternary ammonium salt is calculated according to the mass ratio of the chitosan quaternary ammonium salt to the microcapsule, namely: the phase change microcapsule is 2:1, the non-volatile content of the microcapsule slurry is 40%, stirring is carried out for 30min at 800rpm, an organic silicon defoamer is added for defoaming, and then the chitosan quaternary ammonium salt is uniformly coated on the surface of the phase change microcapsule by a spray drying process, wherein the spray drying conditions are as follows: the air inlet temperature is 180 ℃; the air outlet temperature is 92 ℃; the air pressure is 0.3 MPa; the obtained powder is the surface modified capsule.

b. Preparation of Capsule-containing Fabric

Mixing 35 parts of surface-modified capsule powder, 4 parts of epichlorohydrin crosslinking agent, 3 parts of sodium polyacrylate thickener, 0.1 part of JFC penetrating agent, 0.1 part of mineral oil defoaming agent and 57.8 parts of pure water, stirring at 1000rpm for 10min until the viscosity is more than 8000cps, and discharging; then preparing temperature-adjusting fabric by using the prepared capsule finishing slurry through a rotary screen printing process, wherein the fabric is modal, a machine roller magnetic bar No. 16, the speed of the machine is 20 yards, the drying temperature is 135 ℃, the printed coating is kept for about 3min in a hot air drying oven, and finally, the temperature-adjusting fabric is sequentially subjected to water washing and 180 ℃ heat setting treatment; thus obtaining the capsule-containing fabric of the invention.

Example 3

a. Preparation of capsules

Firstly, dissolving chitosan quaternary ammonium salt in pure water at 60 ℃ under stirring at 100rpm to prepare a chitosan quaternary ammonium salt solution with the mass fraction of 8%; slowly adding the chitosan quaternary ammonium salt solution into the phase-change microcapsule slurry which is dispersed in advance, wherein the dosage of the chitosan quaternary ammonium salt is calculated according to the mass ratio of the chitosan quaternary ammonium salt to the microcapsule, namely: the phase change microcapsule is 2.5:1, the non-volatile content of the microcapsule slurry is 40%, stirring is carried out for 30min at 800rpm, an organic silicon defoamer is added for defoaming, and then the chitosan quaternary ammonium salt is uniformly coated on the surface of the phase change microcapsule by a spray drying process, wherein the spray drying conditions are as follows: the inlet air temperature is 185 ℃; the air outlet temperature is 95 ℃; the air pressure is 0.4 MPa; the obtained powder is the surface modified capsule.

b. Preparation of Capsule-containing Fabric

Mixing 55 parts of surface-modified capsule powder, 10 parts of aluminum oxide heat-conducting filler, 10 parts of epichlorohydrin crosslinking agent, 2 parts of sodium polyacrylate thickener, 0.1 part of JFC penetrating agent, 0.2 part of mineral oil defoaming agent and 22.7 parts of pure water, stirring at 1000rpm for 10min until the viscosity is more than 8000cps, and discharging; then preparing the prepared capsule finishing slurry into temperature-adjusting fabric through a rotary screen printing process, wherein the fabric is viscose fabric, a machine roller magnetic bar No. 16, the speed of the machine is 20 yards, the drying temperature is 135 ℃, the printed coating is ensured to be kept in a hot air drying oven for about 3.5min, and finally, the temperature-adjusting fabric is sequentially subjected to water washing and 185 ℃ heat setting treatment; thus obtaining the capsule-containing fabric of the invention.

Example 4

a. Preparation of capsules

Firstly, dissolving chitosan quaternary ammonium salt in pure water at 60 ℃ under stirring at 100rpm to prepare a chitosan quaternary ammonium salt solution with the mass fraction of 8%; slowly adding the chitosan quaternary ammonium salt solution into the phase-change microcapsule slurry which is dispersed in advance, wherein the dosage of the chitosan quaternary ammonium salt is calculated according to the mass ratio of the chitosan quaternary ammonium salt to the microcapsule, namely: the phase change microcapsule is 3:1, the nonvolatile content of the microcapsule slurry is 40%, stirring is carried out for 30min at 800rpm, mineral oil defoaming agents are added for defoaming, and then chitosan quaternary ammonium salt is uniformly coated on the surface of the phase change microcapsule by an airflow spray drying process, wherein the spray drying conditions are as follows: the air inlet temperature is 190 ℃; the air outlet temperature is 97 ℃; the air pressure is 0.5 MPa; the obtained powder is the surface modified capsule.

b. Preparation of Capsule-containing Fabric

Mixing 65 parts of surface-modified capsule powder, 10 parts of sodium tripolyphosphate cross-linking agent, 2 parts of sodium polyacrylate thickener, 0.1 part of JFC penetrating agent, 0.2 part of organosilicon defoaming agent and 22.7 parts of pure water, stirring at 1000rpm for 10min until the viscosity is more than 8000cps, and discharging; then preparing temperature-adjusting fabric by using the prepared capsule finishing slurry through a rotary screen printing process, wherein the fabric is pure cotton knitted fabric, a machine roller magnetic rod No. 16, the vehicle speed of 20 yards and the drying temperature of 135 ℃ ensure that a printing coating is kept for about 4min in a hot air drying oven, and finally, washing and heat setting at 190 ℃ are carried out in sequence; thus obtaining the capsule-containing fabric of the invention.

Comparative example

(1) Preparation of common phase-change microcapsule powder

Slowly adding pure water into the phase-change microcapsule slurry which is dispersed in advance, wherein the using amount of the pure water is calculated according to the mass ratio of the pure water to the microcapsules, namely the pure water: the phase change microcapsule is 2:1, the nonvolatile content of the microcapsule slurry is 40%, stirring is carried out for 30min at 800rpm, mineral oil defoaming agent is added for defoaming, and then common phase change microcapsule powder is prepared by a spray drying method under the spray drying conditions that: the air inlet temperature is 180 ℃; the air outlet temperature is 90 ℃; the air pressure is 0.3 MPa; the obtained powder is the common phase-change microcapsule powder.

(2) Preparation of thermoregulated Fabric

Mixing 50 parts of common microcapsule powder subjected to spray drying treatment, 6 parts of aziridine cross-linking agent, 3 parts of sodium polyacrylate thickener, 0.1 part of JFC penetrating agent, 0.1 part of organosilicon defoaming agent and 40.8 parts of pure water, stirring at 1000rpm for 10min until the viscosity is more than 8000cps, and discharging; then preparing the prepared phase-change microcapsule finishing slurry into a temperature-regulating fabric by a rotary screen printing process, wherein the fabric is a pure cotton knitted fabric, a machine roller magnetic bar No. 16, the vehicle speed of 20 yards and the drying temperature of 135 ℃ ensure that a printing coating is kept in a hot air oven for about 3min, and finally, washing and heat setting at 180 ℃ are carried out in sequence; and obtaining the temperature-regulating fabric based on the unmodified phase-change microcapsules.

The performance test of the temperature-regulating fabrics obtained in examples 1 to 4 and the comparative example was carried out by the following test methods:

enthalpy of heatValue test method: n is a radical of₂The temperature is increased from 0 ℃ to 60 ℃ at the temperature of 3 ℃/min, the temperature is kept for 2min, and then the temperature is reduced from 60 ℃ to 0 ℃, and the testing instrument is DSC25 of American TA company.

Washing test method: and (3) carrying out washing resistance test according to a washing fastness test standard GBT 8629 and 2017 household washing and drying program for textile test, wherein the enthalpy loss rate calculation mode is a percentage of the difference of the measured fusion enthalpy values before and after washing and the fusion enthalpy value ratio before washing.

The test results were as follows:

according to the test results, the melting enthalpy value of the temperature-adjusting fabric prepared by the method is still maintained to be 84-92% of that after the temperature-adjusting fabric is washed for 20 times, the melting enthalpy value of a comparative example not containing the surface-modified microcapsule is only maintained to be about 16% of that after the temperature-adjusting fabric is finished, and the phase-change material is greatly lost. In addition, the capsule surface modification method adopted by the invention is a physical spray drying method, does not limit the application of the types of the surface active groups of the capsule wall materials, and has very wide application prospect.

The present invention and its embodiments have been described above schematically, without limitation, and what is shown in the drawings is only one of the embodiments of the present invention, and the actual structure is not limited thereto. Therefore, if the person skilled in the art receives the teaching, without departing from the spirit of the invention, the person skilled in the art shall not inventively design the similar structural modes and embodiments to the technical solution, but shall fall within the scope of the invention.