阅读说明：本技术 一种吸湿放热与相变调温结合的复合面料及其制备方法 (Composite fabric combining moisture absorption, heat release and phase change temperature adjustment and preparation method thereof ) 是由 张志成 张丽 马晓飞 于 2021-06-29 设计创作，主要内容包括：本发明公开了一种吸湿放热与相变调温结合的复合面料及其制备方法,涉及面料加工技术领域,所述复合面料由聚丙烯腈和功能化微胶囊制成,功能化微胶囊的壁材为水性环氧树脂,芯材为相变材料。本发明通过功能化微胶囊的添加使所制面料兼具吸湿放热与相变调温的双重功能,其中吸湿放热功能可以增强面料的保暖效果,满足FZ/T 73036-2010的标准要求；相变调温功能具有双向温度调节作用,使面料保持在一个舒适的温度范围,两种功能的复合可以显著改善面料的穿着舒适性,进而提高面料的市场竞争力。(The invention discloses a composite fabric combining moisture absorption, heat release and phase change and temperature adjustment and a preparation method thereof, and relates to the technical field of fabric processing. According to the invention, the prepared fabric has dual functions of moisture absorption, heat release and phase change and temperature regulation by adding the functional microcapsules, wherein the moisture absorption and heat release functions can enhance the warm-keeping effect of the fabric and meet the standard requirements of FZ/T73036-; the phase-change temperature-regulating function has a bidirectional temperature-regulating effect, so that the fabric is kept in a comfortable temperature range, the wearing comfort of the fabric can be obviously improved by combining the two functions, and the market competitiveness of the fabric is further improved.)

1. The composite fabric combining moisture absorption, heat release and phase change temperature adjustment is characterized in that: the material is prepared from polyacrylonitrile and functionalized microcapsules, wherein the wall material of the functionalized microcapsules is water-based epoxy resin, and the core material is a phase-change material; the waterborne epoxy resin is prepared from epoxy resin and a silane coupling agent KH550, the molar ratio of the epoxy resin to the silane coupling agent KH550 is (2-5):1, and the molar weight of the epoxy resin is calculated by epoxy groups.

2. The composite fabric according to claim 1, wherein: the mass ratio of the polyacrylonitrile to the functionalized microcapsule is (90-99) to (1-10).

3. The composite fabric according to claim 1, wherein: the mass ratio of the waterborne epoxy resin to the phase-change material is 1-10: 1.

4. The composite fabric according to claim 1, wherein: the phase-change material is at least one of paraffin, lauric acid and octadecane.

5. The composite fabric according to claim 1, wherein: the grain diameter of the functionalized microcapsule is 5-20 μm.

6. The composite fabric according to claim 1, wherein: the preparation method of the water-based epoxy resin comprises the steps of dissolving the epoxy resin in acetone, adding the silane coupling agent KH550, heating to reflux under stirring, carrying out heat preservation reaction, stopping the reaction after the silane coupling agent KH550 completely reacts, carrying out reduced pressure distillation to remove the acetone, and carrying out vacuum drying on the remainder to obtain the water-based epoxy resin.

7. A method of making a composite fabric as claimed in any one of claims 1 to 6, comprising the steps of:

(1) adding a phase change material and an emulsifier into deionized water, and emulsifying to obtain a core material solution;

(2) dissolving water-based epoxy resin in acetone to obtain a wall material solution;

(3) dropwise adding the core material solution into the wall material solution, adding a curing agent, heating and stirring until acetone is completely volatilized, filtering, washing and drying to obtain a functionalized microcapsule;

(4) adding polyacrylonitrile into dimethylformamide, and dissolving to obtain a spinning solution;

(5) adding the functionalized microcapsules into the spinning solution, uniformly mixing, extruding through a spinneret orifice, solidifying and forming in a solidification bath, hot drawing, washing with water, drying, spinning and weaving to obtain the composite fabric.

8. The method for preparing a composite fabric according to claim 7, characterized in that: the emulsifier is at least one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and Tween; the mass concentration of the emulsifier in the core material solution is 1-10%.

9. The method for preparing a composite fabric according to claim 7, characterized in that: the curing agent is at least one of ethylenediamine, diethylenetriamine and triethylene tetramine.

10. The method for preparing a composite fabric according to claim 7, characterized in that: the mass ratio of the waterborne epoxy resin to the curing agent is 100 (5-15).

The technical field is as follows:

the invention relates to the technical field of fabric processing, in particular to a composite fabric combining moisture absorption, heat release and phase change temperature adjustment and a preparation method thereof.

Background art:

the heating fiber comprises moisture absorption heating fiber, light energy heating fiber, phase change material, chemical heat release material and electric energy heating material, and is a positive heat generation type warm-keeping material.

The moisture absorption heating fiber has a large amount of hydrophilic groups, is good in moisture absorption and heating performance, and can release heat while absorbing moisture. The natural fibers have certain moisture absorption and heat generation performances, the moisture absorption and heat generation effects of wool are particularly obvious, but wool has the defects of shrinkage, wrinkling and easy deformation.

The phase-change fiber is a heat-storage temperature-regulating functional fiber developed by utilizing the characteristics of releasing or absorbing latent heat and keeping constant temperature in the phase-change process of a substance. When the ambient temperature or the skin temperature of a human body reaches the melting point of the phase-change material in the garment, the phase-change material absorbs heat and is converted from a solid state to a liquid state, and therefore a short-term refrigeration effect is generated in the inner layer of the garment. The heat energy may come from the external warm environment or from the human body itself, and once the phase change material is completely melted, the energy storage is finished. If the garment is used in a cold environment below the crystallization temperature of the phase change material, the temperature of the garment will be below the phase change temperature, at which point the liquid phase change material will change back to a solid state, releasing its stored energy, providing a transient heating effect.

The invention combines two heating modes of moisture absorption and heat release and phase change temperature regulation, provides a preparation method of the composite fabric, and can store or release heat according to the change of environment and human body temperature, thereby improving the wearing comfort of the fabric.

The invention content is as follows:

the invention aims to solve the technical problem of providing a composite fabric combining moisture absorption, heat release and phase change temperature regulation and a preparation method thereof.

The technical problem to be solved by the invention is realized by adopting the following technical scheme:

the invention provides a composite fabric combining moisture absorption, heat release and phase change temperature regulation, which is prepared from polyacrylonitrile and functional microcapsules, wherein the wall material of the functional microcapsules is water-based epoxy resin, and the core material is a phase change material;

the waterborne epoxy resin is prepared from epoxy resin and a silane coupling agent KH550, the molar ratio of the epoxy resin to the silane coupling agent KH550 is (2-5):1, and the molar weight of the epoxy resin is calculated by epoxy groups.

The mass ratio of the polyacrylonitrile to the functionalized microcapsule is (90-99) to (1-10).

The mass ratio of the waterborne epoxy resin to the phase-change material is 1-10: 1.

The phase-change material is at least one of paraffin, lauric acid and octadecane. Alternative phase change materials are not limited thereto, and n-alkanes of C14-C30, fatty acids of C8-C18, and esters thereof can also be used as the phase change material.

The grain diameter of the functionalized microcapsule is 5-20 μm.

The preparation method of the water-based epoxy resin comprises the steps of dissolving the epoxy resin in acetone, adding the silane coupling agent KH550, heating to reflux under stirring, carrying out heat preservation reaction, stopping the reaction after the silane coupling agent KH550 completely reacts, carrying out reduced pressure distillation to remove the acetone, and carrying out vacuum drying on the remainder to obtain the water-based epoxy resin.

Because the structure of the epoxy resin molecule contains epoxy group, and the structure of the silane coupling agent KH550 molecule contains amino group and siloxy group, under the heating condition, the epoxy group can quickly react with the amino group, and the epoxy group generates hydroxyl group through ring opening, so that the hydroxyl group and the siloxy group are introduced into the structure of the epoxy resin molecule. The existence of hydroxyl can improve the hydrophilicity of the epoxy resin, so that the moisture absorption performance of the wall material is enhanced; the existence of the silicon oxygen group can improve the mechanical strength and the high temperature resistance of the epoxy resin, thereby enhancing the encapsulation performance and the heat resistance of the wall material.

The invention also provides a preparation method of the composite fabric, which comprises the following steps:

(1) adding a phase change material and an emulsifier into deionized water, and emulsifying to obtain a core material solution;

(2) dissolving water-based epoxy resin in acetone to obtain a wall material solution;

(3) dropwise adding the core material solution into the wall material solution, adding a curing agent, heating and stirring until acetone is completely volatilized, filtering, washing and drying to obtain a functionalized microcapsule;

(4) adding polyacrylonitrile into dimethylformamide, and dissolving to obtain a spinning solution;

(5) adding the functionalized microcapsules into the spinning solution, uniformly mixing, extruding through a spinneret orifice, solidifying and forming in a solidification bath, hot drawing, washing with water, drying, spinning and weaving to obtain the composite fabric.

The emulsifier is at least one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and Tween.

The mass concentration of the emulsifier in the core material solution is 1-10%.

The curing agent is at least one of ethylenediamine, diethylenetriamine and triethylene tetramine. The curing agent is added to promote the curing of the epoxy resin and form a stable encapsulation structure for the core material.

The mass ratio of the waterborne epoxy resin to the curing agent is 100 (5-15).

The water-based epoxy resin is selected as the wall material of the functional microcapsule, on one hand, the existence of hydroxyl in the structure of the water-based epoxy resin can capture water molecules moving in the air, the water molecules are adsorbed on the surface of the fiber, and the kinetic energy of the water molecules is converted into heat, so that the effects of moisture absorption and heat release are exerted; on the other hand, the cured epoxy resin can play a good role in encapsulating the core material, has good heat resistance, and can ensure that the phase-change material can efficiently and stably play a role in regulating the temperature.

The phase change material is N-ethyl succinimide.

N-ethylsuccinimide is selected as a phase-change material for optimizing the phase-change temperature-adjusting function of the fabric, but the prior art in the field does not disclose N-ethylsuccinimide as the phase-change material, and the common general knowledge in the field does not give technical inspiration of N-ethylsuccinimide as the phase-change material, but the invention realizes the new application of N-ethylsuccinimide as the phase-change material and obtains the effect superior to paraffin, lauric acid and octadecane.

The invention has the beneficial effects that: the fabric prepared by the method has dual functions of moisture absorption and heat release and phase change and temperature regulation by adding the functional microcapsules, wherein the moisture absorption and heat release functions can enhance the heat preservation effect of the fabric, the maximum temperature rise value exceeds 4 ℃, the average temperature rise value exceeds 3 ℃ within 30min, and the standard requirement of FZ/T73036-; the phase-change temperature-regulating function has a bidirectional temperature-regulating effect, so that the fabric is kept in a comfortable temperature range, the wearing comfort of the fabric can be obviously improved by combining the two functions, and the market competitiveness of the fabric is further improved.

The specific implementation mode is as follows:

in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.

Example 1

1. Preparation of the waterborne epoxy resin:

dissolving epoxy resin E51 in acetone, adding silane coupling agent KH550, wherein the molar ratio of epoxy resin to silane coupling agent KH550 is 4:1, heating under stirring to reflux, keeping the temperature for reaction, stopping reaction after the silane coupling agent KH550 completely reacts, distilling under reduced pressure to remove acetone, and vacuum-drying the remainder to obtain the water-based epoxy resin.

2. Preparing a composite fabric:

(1) adding 35# paraffin and sodium dodecyl benzene sulfonate into deionized water, and emulsifying to obtain a core material solution, wherein the mass concentration of the emulsifier in the core material solution is 5%.

(2) And dissolving the water-based epoxy resin in acetone to obtain a wall material solution.

(3) Dropwise adding the core material solution into the wall material solution, adding diethylenetriamine, heating and stirring until acetone is completely volatilized, filtering, washing and drying to obtain the functionalized microcapsule with the average particle size of 15.8 mu m, wherein the mass ratio of the waterborne epoxy resin to the 35# paraffin is 5:1, and the mass ratio of the waterborne epoxy resin to the curing agent is 100: 10.

(4) Adding polyacrylonitrile into dimethylformamide, and dissolving to obtain spinning solution.

(5) Adding the functionalized microcapsule into the spinning solution, wherein the mass ratio of polyacrylonitrile to the functionalized microcapsule is 95:5, uniformly mixing, extruding through a spinneret orifice, solidifying and forming in a coagulating bath, hot drawing, washing with water, drying, spinning and weaving to obtain the composite fabric.

Example 2

1. Preparation of the waterborne epoxy resin:

dissolving epoxy resin E44 in acetone, adding silane coupling agent KH550, wherein the molar ratio of epoxy resin to silane coupling agent KH550 is 4:1, heating under stirring to reflux, keeping the temperature for reaction, stopping reaction after the silane coupling agent KH550 completely reacts, distilling under reduced pressure to remove acetone, and vacuum-drying the remainder to obtain the water-based epoxy resin.

2. Preparing a composite fabric:

(1) adding lauric acid and tween 60 into deionized water, and emulsifying to obtain a core material solution, wherein the mass concentration of the emulsifier in the core material solution is 8%.

(2) And dissolving the water-based epoxy resin in acetone to obtain a wall material solution.

(3) Dropwise adding the core material solution into the wall material solution, wherein the mass ratio of the waterborne epoxy resin to the lauric acid is 4:1, adding triethylene tetramine, the mass ratio of the waterborne epoxy resin to the curing agent is 100:10, heating and stirring until acetone is completely volatilized, filtering, washing and drying to obtain the functionalized microcapsule with the average particle size of 13.5 microns.

(4) Adding polyacrylonitrile into dimethylformamide, and dissolving to obtain spinning solution.

(5) Adding the functionalized microcapsule into the spinning solution, wherein the mass ratio of polyacrylonitrile to the functionalized microcapsule is 94:6, uniformly mixing, extruding through a spinneret orifice, solidifying and forming in a coagulating bath, hot drawing, washing with water, drying, spinning and weaving to obtain the composite fabric.

Example 3

1. Preparation of the waterborne epoxy resin:

dissolving epoxy resin E51 in acetone, adding silane coupling agent KH550, wherein the molar ratio of epoxy resin to silane coupling agent KH550 is 3:1, heating under stirring to reflux, keeping the temperature for reaction, stopping reaction after the silane coupling agent KH550 completely reacts, distilling under reduced pressure to remove acetone, and vacuum-drying the remainder to obtain the water-based epoxy resin.

2. Preparing a composite fabric:

(1) adding octadecane and sodium dodecyl sulfate into deionized water, and emulsifying to obtain a core material solution, wherein the mass concentration of the emulsifier in the core material solution is 10%.

(2) And dissolving the water-based epoxy resin in acetone to obtain a wall material solution.

(3) Dropwise adding the core material solution into the wall material solution, wherein the mass ratio of the waterborne epoxy resin to the octadecane is 3:1, adding diethylenetriamine, the mass ratio of the waterborne epoxy resin to the curing agent is 100:12, heating and stirring until the acetone is completely volatilized, filtering, washing and drying to obtain the functionalized microcapsule with the average particle size of 14.2 microns.

(4) Adding polyacrylonitrile into dimethylformamide, and dissolving to obtain spinning solution.

(5) Adding the functionalized microcapsule into the spinning solution, wherein the mass ratio of polyacrylonitrile to the functionalized microcapsule is 95:5, uniformly mixing, extruding through a spinneret orifice, solidifying and forming in a coagulating bath, hot drawing, washing with water, drying, spinning and weaving to obtain the composite fabric.

Example 4

Example 4 the same procedure as in example 1 was repeated except that the 35# paraffin wax in example 1 was replaced with N-ethylsuccinimide of equal mass.

Comparative example

Comparative example the procedure of example 1 was followed except that the aqueous epoxy resin of example 1 was replaced with an equal mass of a commercially available aqueous epoxy resin EPIKOTE WD-510A.

The moisture absorption and heat release performance of the composite fabric is tested according to the standard FZ/T73036-2010, the phase change and temperature regulation performance of the composite fabric is tested by adopting differential scanning calorimetry, and the test results are shown in Table 1.

TABLE 1

	Maximum rise temperature value/. degree.C	Average temperature rise/deg.C within 30min	Phase transition temperature/. degree.C	Enthalpy of phase change J/g
					Example 1	5.4	3.2	15-38	126
Example 2	5.7	3.4	18-42	140
					Example 3	6.0	3.5	20-36	135
Example 4	6.5	3.7	15-40	147
					Comparative example	3.2	1.3	18-35	112

The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.