阅读说明：本技术 一种耐水洗棉织物控温整理剂的制备方法 (Preparation method of temperature control finishing agent for washable cotton fabric ) 是由 雷洪军 于 2021-01-14 设计创作，主要内容包括：本发明涉及一种耐水洗棉织物控温整理剂的制备方法,属于纺织材料技术领域,本发明通过聚丙烯酸酯包覆正十八烷相变微胶囊为原料,制备一种耐水洗棉织物控温整理剂通过微胶囊技术,相变材料的比表面积能够明显增大,相分离和过冷得到消除,耐久性、使用寿命得到提高,在较长的时间内,防止芯材泄漏,本发明以水性环氧乳液为整理剂基料,制备一种耐水洗棉织物控温整理剂,水性环氧乳液中的环氧树脂结构中含有极其活泼的环氧基、醚键和羟基,环氧基团可以与棉织物和无机物阻燃剂的表面形成化学键,而羟基和醚键有极高的极性,使得环氧树脂与相邻界面产生电磁吸力,环氧树脂具有特别强的粘合力,可以有效提高控温整理剂的耐水洗牢度。(The invention relates to a preparation method of a temperature control finishing agent for washable cotton fabrics, which belongs to the technical field of textile materials, and the invention prepares the temperature control finishing agent for washable cotton fabrics by using a polyacrylate coated octadecane phase change microcapsule as a raw material and using a microcapsule technology, wherein the specific surface area of the phase change material can be obviously increased, phase separation and supercooling can be eliminated, the durability and the service life can be improved, and core material leakage can be prevented within a longer time. The epoxy resin has extremely strong adhesive force, and can effectively improve the washing fastness of the temperature-control finishing agent.)

1. A preparation method of a temperature control finishing agent for washable cotton fabrics is characterized by comprising the following specific preparation steps:

(1) adding the aqueous epoxy emulsion, polyethylene glycol and polyvinyl alcohol into absolute ethyl alcohol, and stirring at the normal temperature at the rotating speed of 200-240 r/min for 20-30 min to obtain a polymer ethanol solution;

(2) adding octyl phenol polyoxyethylene ether and sodium dodecyl sulfate into deionized water, stirring for 10-12 min at the rotating speed of 300-400 r/min under the water bath condition of 40-60 ℃, and preserving heat to obtain an emulsifier solution;

(3) adding the modified heat-storage temperature-regulating phase-change microcapsule, a polymer ethanol solution and hydroxypropyl silicone oil into an emulsifier solution, placing the mixture into a high-speed stirrer, stirring the mixture for 40-60 min at the rotating speed of 4000-6000 r/min under the water bath condition of 40-60 ℃, placing the mixture into an ultrasonic dispersion machine, and performing ultrasonic dispersion for 20-30 min at normal temperature to obtain the temperature-control finishing agent for the washable cotton fabric.

2. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 1, wherein the modified heat-storage temperature-regulation phase-change microcapsule, the aqueous epoxy emulsion, the absolute ethyl alcohol, the polyethylene glycol, the polyvinyl alcohol, the hydroxypropyl silicone oil, the polyoxyethylene octylphenol ether, the sodium dodecyl sulfate and the deionized water are respectively 20-40 parts by weight of the modified heat-storage temperature-regulation phase-change microcapsule, 16-32 parts by weight of the aqueous epoxy emulsion, 80-160 parts by weight of the absolute ethyl alcohol, 4-8 parts by weight of the polyethylene glycol, 10-20 parts by weight of the polyvinyl alcohol, 8-16 parts by weight of the hydroxypropyl silicone oil, 1-2 parts by weight of the polyoxyethylene octylphenol ether, 0.8-1.6 parts by weight of sodium dodecyl benzene sulfonate and 20-40 parts by weight of the deionized.

3. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 1, wherein the power of ultrasonic dispersion in the step (3) is 400-500W.

4. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 1, wherein the specific preparation steps of the modified heat-storage temperature-regulation phase-change microcapsule in the step (3) are as follows:

(1) adding vinyltriethoxysilane and stearic acid into absolute ethyl alcohol, stirring for 10-20 min at the rotating speed of 260-280 r/min under the water bath condition of 50-60 ℃, and preserving heat to obtain a modified solution;

(2) adding the heat-storage temperature-regulating phase-change microcapsules into the modified liquid, stirring for 30-40 min at a rotating speed of 200-240 r/min under a water bath condition of 40-50 ℃, placing in an ultrasonic dispersion machine, and performing ultrasonic treatment for 20-30 min at normal temperature to obtain a dispersion liquid;

(3) and (3) placing the dispersion liquid in a centrifuge, centrifugally separating at the normal temperature at the rotating speed of 4000-5000 r/min for 10-20 min, taking a lower-layer solid, washing with absolute ethyl alcohol for 3-5 times, placing in an oven at the temperature of 60-80 ℃ for drying for 1-2 h, and cooling at the normal temperature to obtain the modified heat storage temperature regulation phase change microcapsule.

5. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 3, wherein the heat-storage and temperature-regulation phase-change microcapsules, the vinyltriethoxysilane, the stearic acid and the absolute ethyl alcohol are respectively 20-40 parts by weight of the heat-storage and temperature-regulation phase-change microcapsules, 4-8 parts by weight of the vinyltriethoxysilane, 2-4 parts by weight of the stearic acid and 120-240 parts by weight of the absolute ethyl alcohol.

6. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 3, wherein the power of the ultrasonic treatment in the step (2) is 500-600W.

7. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 3, wherein the specific preparation steps of the heat-storage temperature-control phase-change microcapsules in the step (2) are as follows:

(1) adding dodecyl trimethyl ammonium chloride into deionized water, stirring at the normal temperature at the rotating speed of 180-200 r/min for 10-12 min, and adjusting the pH to 5-6 to obtain a dodecyl trimethyl ammonium chloride mixed solution;

(2) adding acrylic acid and ethyl acrylate into vinyl acetate, and stirring and mixing at the rotating speed of 200-240 r/min for 16-20 min at normal temperature to obtain a mixed monomer;

(3) adding a mixed solution of 1/2 mass dodecyl trimethyl ammonium chloride into a mixed monomer, placing the mixed solution into a high-shear emulsifying machine, stirring and emulsifying at the normal temperature at the rotating speed of 10000-14000 r/min for 1-2 h to obtain a mixed emulsion, placing n-octadecane in a water bath condition of 40-50 ℃ for heating for 20-30 min, and preserving heat to obtain n-octadecane liquid;

(4) adding azodiisobutyronitrile and the rest 1/2 mass of dodecyl trimethyl ammonium chloride mixed solution into n-octadecane liquid, placing the mixture into a high-shear emulsifying machine, stirring and emulsifying the mixture for 30-40 min at the rotating speed of 8000-10000 r/min under the water bath condition of 40-60 ℃, and preserving heat to obtain n-octadecane mixed emulsion;

(5) slowly adding the mixed emulsion into the mixed emulsion of n-octadecane, stirring for 1-2 h at the rotating speed of 120-160 r/min under the water bath condition of 70-80 ℃, and standing for 4-6 h under the condition of heat preservation to obtain microcapsule mixed liquid;

(6) and placing the microcapsule mixed solution in a centrifuge, centrifuging and separating at the normal temperature at the rotating speed of 3000-3500 r/min for 20-30 min, taking the lower-layer solid, washing for 3-5 times by using deionized water, placing in an oven, and drying at the temperature of 40-60 ℃ for 20-30 min to obtain the heat-storage temperature-regulating phase-change microcapsule.

8. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 7, wherein the weight parts of the n-octadecane, the acrylic acid, the ethyl acrylate, the vinyl acetate, the dodecyl trimethyl ammonium chloride, the azobisisobutyronitrile and the deionized water are respectively 20-40 parts of the n-octadecane, 12-24 parts of the acrylic acid, 40-80 parts of the ethyl acrylate, 24-48 parts of the vinyl acetate, 8-16 parts of the dodecyl trimethyl ammonium chloride, 0.4-0.8 part of the azobisisobutyronitrile and 120-240 parts of the deionized water.

9. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 7, wherein the pH adjustment in step (1) is performed by using 1% by mass of acetic acid.

10. The preparation method of the temperature-control finishing agent for the washable cotton fabric according to claim 7, wherein the slow adding rate of the mixed emulsion in the step (5) is 20-30 mL/min.

Technical Field

The invention relates to a preparation method of a temperature control finishing agent for washable cotton fabrics, belonging to the technical field of textile materials.

Background

The temperature adjusting effect of the temperature adjusting textile mainly depends on the phase change material in the textile, and the textile has the characteristics of initiative and adaptability to temperature adjustment. The temperature-regulating textile has a plurality of preparation methods, and the temperature-regulating textile is mainly prepared by adding and finishing a temperature-regulating material on the surface of the temperature-regulating textile or directly spinning to prepare temperature-regulating fibers and then spinning or blending. The preparation methods of the temperature-regulating textile can be divided into four categories: hollow fiber processes, spinning processes, foam processes, and post-finishing processes.

The hollow fiber filling method is to fill the phase change material into the hollow part of the hollow fiber and utilize the reversible heat storage function of the phase change material to make the fabric obtain the temperature adjusting performance. However, when the hollow fiber impregnation filling method is adopted to produce the temperature-adjusting fiber, the temperature-adjusting fiber is difficult to popularize in industrial application due to the large diameter of the used fiber. The spinning method is to add phase-change materials into a melt or solution of spinning polymers, and obtain the temperature-regulating fibers containing the phase-change materials after spinning processing. The spinning method includes wet spinning and melt spinning, and the wet spinning is a main method for industrial preparation at present, namely, the phase-change material and the spinning solution are mixed and then spun. The microcapsule can ensure that the phase change material is not easy to leak, plays a certain protection role on the phase change material, and can conveniently use the phase change material in the spinning processing process, so that the durability of the prepared fiber is improved. The microcapsule used in the textile field is prepared by coating a phase change material in a specific temperature range with certain high molecular compounds or inorganic compounds by a physical or chemical method to prepare solid particles (the diameter is 1-100 mu m) which are stable in a normal state. The thermoregulation acrylic fiber is the fiber produced by the solution spinning technology at first. The melt spinning method is to disperse the stable phase-change material in the form of microcapsules in the molten liquid of the polymer, and then to spin the stable phase-change material to prepare the temperature-adjusting fiber. The microcapsules are directly embedded in the fibers, so that the phase change substances in the microcapsules can be stably present in the fibers, but the addition amount of the microcapsules has a certain influence on the tensile strength of the fibers. The difference of the melt spinning method compared with the wet spinning method is that the temperature requirement on the phase-change material is higher, the temperature of the spinning solution is between 200 ℃ and 400 ℃, and the adopted phase-change microcapsule has good thermal stability and chemical stability. The preparation of the temperature-regulating textile by the foam method is to add the temperature-regulating microcapsules into the foam material and to uniformly distribute the microcapsules by the water blowing method. The foam material obtained by the foam method is softer, the weight gain rate of the microcapsule can reach 48%, but the strength is greatly reduced. The post-finishing preparation method is a method for applying a phase-change material to a fabric by means of padding finishing or coating, so as to obtain the temperature-regulating textile. After finishing, the hand feeling of the fabric is reduced, the fastness to washing of the phase change material is low, and abrasion can easily occur in the washing process.

Disclosure of Invention

The technical problems to be solved by the invention are as follows: aiming at the problems that the existing temperature-regulating finishing agent for cotton fabrics has low fastness to washing and is easy to wear in the washing process, the preparation method of the temperature-regulating finishing agent for the cotton fabrics resistant to washing is provided.

In order to solve the technical problems, the invention adopts the technical scheme that:

(1) adding the aqueous epoxy emulsion, polyethylene glycol and polyvinyl alcohol into absolute ethyl alcohol, and stirring at the normal temperature at the rotating speed of 200-240 r/min for 20-30 min to obtain a polymer ethanol solution;

(2) adding octyl phenol polyoxyethylene ether and sodium dodecyl sulfate into deionized water, stirring for 10-12 min at the rotating speed of 300-400 r/min under the water bath condition of 40-60 ℃, and preserving heat to obtain an emulsifier solution;

(3) adding the modified heat-storage temperature-regulating phase-change microcapsule, a polymer ethanol solution and hydroxypropyl silicone oil into an emulsifier solution, placing the mixture into a high-speed stirrer, stirring the mixture for 40-60 min at the rotating speed of 4000-6000 r/min under the water bath condition of 40-60 ℃, placing the mixture into an ultrasonic dispersion machine, and performing ultrasonic dispersion for 20-30 min at normal temperature to obtain the temperature-control finishing agent for the washable cotton fabric.

The modified heat-storage temperature-regulating phase-change microcapsule, the water-based epoxy emulsion, the absolute ethyl alcohol, the polyethylene glycol, the polyvinyl alcohol, the hydroxypropyl silicone oil, the octyl phenol polyoxyethylene ether, the sodium dodecyl sulfate and the deionized water are respectively prepared from the following components in parts by weight: 20-40 parts of modified heat-storage temperature-regulating phase-change microcapsules, 16-32 parts of aqueous epoxy emulsion, 80-160 parts of absolute ethyl alcohol, 4-8 parts of polyethylene glycol, 10-20 parts of polyvinyl alcohol, 8-16 parts of hydroxypropyl silicone oil, 1-2 parts of octylphenol polyoxyethylene ether, 0.8-1.6 parts of sodium dodecyl sulfate and 20-40 parts of deionized water.

The power of ultrasonic dispersion is 400-500W.

The specific preparation steps of the modified heat-storage temperature-regulating phase-change microcapsule are as follows

(1) Adding vinyltriethoxysilane and stearic acid into absolute ethyl alcohol, stirring for 10-20 min at the rotating speed of 260-280 r/min under the water bath condition of 50-60 ℃, and preserving heat to obtain a modified solution;

(2) adding the heat-storage temperature-regulating phase-change microcapsules into the modified liquid, stirring for 30-40 min at a rotating speed of 200-240 r/min under a water bath condition of 40-50 ℃, placing in an ultrasonic dispersion machine, and performing ultrasonic treatment for 20-30 min at normal temperature to obtain a dispersion liquid;

(3) and (3) placing the dispersion liquid in a centrifuge, centrifugally separating at the normal temperature at the rotating speed of 4000-5000 r/min for 10-20 min, taking a lower-layer solid, washing with absolute ethyl alcohol for 3-5 times, placing in an oven at the temperature of 60-80 ℃ for drying for 1-2 h, and cooling at the normal temperature to obtain the modified heat storage temperature regulation phase change microcapsule.

The heat storage and temperature regulation phase change microcapsule, the vinyl triethoxysilane, the stearic acid and the absolute ethyl alcohol are respectively in parts by weight: 20-40 parts of heat storage and temperature regulation phase change microcapsules, 4-8 parts of vinyltriethoxysilane, 2-4 parts of stearic acid and 120-240 parts of absolute ethyl alcohol.

The power of ultrasonic treatment is 500-600W.

The heat-storage temperature-regulating phase-change microcapsule comprises the following specific preparation steps:

(1) adding dodecyl trimethyl ammonium chloride into deionized water, stirring at the normal temperature at the rotating speed of 180-200 r/min for 10-12 min, and adjusting the pH to 5-6 to obtain a dodecyl trimethyl ammonium chloride mixed solution;

(2) adding acrylic acid and ethyl acrylate into vinyl acetate, and stirring and mixing at the rotating speed of 200-240 r/min for 16-20 min at normal temperature to obtain a mixed monomer;

(3) adding a mixed solution of 1/2 mass dodecyl trimethyl ammonium chloride into a mixed monomer, placing the mixed monomer in a high-shear emulsifying machine, and stirring and emulsifying at the rotation speed of 10000-14000 r/min for 1-2 hours at normal temperature to obtain a mixed emulsion; placing n-octadecane in a water bath at 40-50 ℃ for heating for 20-30 min, and preserving heat to obtain n-octadecane liquid;

(4) adding azodiisobutyronitrile and the rest 1/2 mass of dodecyl trimethyl ammonium chloride mixed solution into n-octadecane liquid, placing the mixture into a high-shear emulsifying machine, stirring and emulsifying the mixture for 30-40 min at the rotating speed of 8000-10000 r/min under the water bath condition of 40-60 ℃, and preserving heat to obtain n-octadecane mixed emulsion;

(5) slowly adding the mixed emulsion into the mixed emulsion of n-octadecane, stirring for 1-2 h at the rotating speed of 120-160 r/min under the water bath condition of 70-80 ℃, and standing for 4-6 h under the condition of heat preservation to obtain microcapsule mixed liquid;

(6) and placing the microcapsule mixed solution in a centrifuge, centrifuging and separating at the normal temperature at the rotating speed of 3000-3500 r/min for 20-30 min, taking the lower-layer solid, washing for 3-5 times by using deionized water, placing in an oven, and drying at the temperature of 40-60 ℃ for 20-30 min to obtain the heat-storage temperature-regulating phase-change microcapsule.

The n-octadecane, the acrylic acid, the ethyl acrylate, the vinyl acetate, the dodecyl trimethyl ammonium chloride, the azobisisobutyronitrile and the deionized water respectively have the following parts by weight: 20-40 parts of n-octadecane, 12-24 parts of acrylic acid, 40-80 parts of ethyl acrylate, 24-48 parts of vinyl acetate, 8-16 parts of dodecyl trimethyl ammonium chloride, 0.4-0.8 part of azobisisobutyronitrile and 120-240 parts of deionized water.

The pH value is adjusted by adopting acetic acid with the mass fraction of 1 percent.

The slow adding speed of the mixed emulsion is 20-30 mL/min.

Compared with other methods, the method has the beneficial technical effects that:

(1) the invention prepares a temperature control finishing agent for washable cotton fabric by using polyacrylate coated n-octadecane phase change microcapsule as raw material, the microcapsule technology is a technology of coating solid or liquid material with a film forming material to obtain particles with core-shell structure, the capsule wall provides a stable closed environment for the phase change material, which can enhance the stability of the phase change material, and simultaneously can convert solid-liquid phase change into quasi solid-solid phase change, so that the compounding of the phase change material with fiber and textile becomes easy, the phase change material has better heat conductivity because of being dispersed into small particles, by the microcapsule technology, the specific surface area of the phase change material can be obviously increased, phase separation and supercooling are eliminated, the durability and the service life are improved, the phase change microcapsule has core-shell structure, can protect core material with specific function, and can be used in a longer time, the phase change microcapsule has many advantages, can improve the heat conductivity coefficient of the phase change material, can widen the phase change temperature range of the phase change material, and improve the durability of the phase change material;

(2) the invention takes water epoxy emulsion as a finishing agent base material to prepare a temperature control finishing agent for washable cotton fabrics, the epoxy resin structure in the water epoxy emulsion contains extremely active epoxy group, ether bond and hydroxyl group, the epoxy group can form chemical bond with the surfaces of cotton fabrics and inorganic fire retardants, and the hydroxyl group and the ether bond have extremely high polarity, so that the epoxy resin and an adjacent interface generate electromagnetic suction force, therefore, the epoxy resin has extremely strong adhesive force, inorganic flame-retardant microcapsules can be effectively fixed on the surface of the cotton fabrics, the curing reaction of the epoxy resin is mainly epoxy group ring-opening addition curing, no bubble is generated in the curing process, no micromolecule is generated, so the curing shrinkage rate of the epoxy resin is low, the cured epoxy resin only contains benzene ring, ether bond and compact matter with a three-dimensional cross-linking structure, therefore, the chemical stability is good, high mechanical strength and low water absorption, and can effectively improve the fastness to washing of the temperature-control finishing agent.

Detailed Description

Respectively weighing 20-40 parts by weight of n-octadecyl, 12-24 parts by weight of acrylic acid, 40-80 parts by weight of ethyl acrylate, 24-48 parts by weight of vinyl acetate, 8-16 parts by weight of dodecyl trimethyl ammonium chloride, 0.4-0.8 part by weight of azobisisobutyronitrile and 120-240 parts by weight of deionized water, adding dodecyl trimethyl ammonium chloride into deionized water, stirring at a rotating speed of 180-200 r/min for 10-12 min at normal temperature, dropwise adding 1% by mass of acetic acid to adjust the pH to 5-6 to obtain a dodecyl trimethyl ammonium chloride mixed solution, adding acrylic acid and ethyl acrylate into vinyl acetate, stirring and mixing at a rotating speed of 200-240 r/min at normal temperature for 16-20 min to obtain a mixed monomer, adding 1/2 parts by mass of dodecyl trimethyl ammonium chloride mixed solution into the mixed monomer, placing in a high-shear emulsifying machine, stirring and emulsifying at a rotating speed of 10000-14000 r/min at normal temperature for 1-2 h, obtaining mixed emulsion, placing n-octadecane in a water bath condition of 40-50 ℃ for heating for 20-30 min, preserving heat to obtain n-octadecane liquid, adding azodiisobutyronitrile and the rest of the mixed solution of the dodecyltrimethylammonium chloride with the mass of 1/2 into the n-octadecane liquid, placing the mixed solution in a high-shear emulsifying machine, stirring and emulsifying for 30-40 min at the water bath condition of 40-60 ℃ at the rotating speed of 8000-10000 r/min, preserving heat to obtain n-octadecane mixed emulsion, slowly adding the mixed emulsion into the n-octadecane mixed emulsion at the dropping speed of 20-30 mL/min, stirring for 1-2 h at the rotating speed of 120-160 r/min at the water bath condition of 70-80 ℃, preserving heat for 4-6 h to obtain microcapsule mixed liquid, placing the microcapsule mixed liquid in a centrifugal machine, centrifugally separating for 20-30 min at the rotating speed of 3000-3500 r/min at normal temperature, taking lower layer solid, washing with deionized water for 3-5 times, placing in an oven, and drying at 40-60 ℃ for 20-30 min to obtain a heat storage temperature regulation phase change microcapsule;

respectively weighing 20-40 parts of heat storage and temperature regulation phase change microcapsules, 4-8 parts of vinyltriethoxysilane, 2-4 parts of stearic acid and 120-240 parts of absolute ethanol, adding the vinyltriethoxysilane and the stearic acid into the absolute ethanol, stirring for 10-20 min at a rotating speed of 260-280 r/min under a water bath condition of 50-60 ℃, preserving heat to obtain a modified solution, adding the heat storage and temperature regulation phase change microcapsules into the modified solution, stirring for 30-40 min at a rotating speed of 200-240 r/min under a water bath condition of 40-50 ℃, placing in an ultrasonic dispersion machine, carrying out ultrasonic treatment for 20-30 min at a power of 500-600W at normal temperature to obtain a dispersion solution, placing the dispersion solution in a centrifuge, carrying out centrifugal separation for 10-20 min at a rotating speed of 4000-5000 r/min at normal temperature, taking a lower layer solid, washing for 3-5 times by using the absolute ethanol, placing in an oven at 60-80 ℃, drying for 1-2 h, cooling at normal temperature to obtain modified heat storage temperature regulation phase change microcapsules;

respectively weighing 20-40 parts by weight of modified heat storage and temperature regulation phase change microcapsules, 16-32 parts by weight of aqueous epoxy emulsion, 80-160 parts by weight of absolute ethyl alcohol, 4-8 parts by weight of polyethylene glycol, 10-20 parts by weight of polyvinyl alcohol, 8-16 parts by weight of hydroxypropyl silicone oil, 1-2 parts by weight of octylphenol polyoxyethylene ether, 0.8-1.6 parts by weight of sodium dodecyl sulfate and 20-40 parts by weight of deionized water, adding the aqueous epoxy emulsion, the polyethylene glycol and the polyvinyl alcohol into the absolute ethyl alcohol, stirring at the rotating speed of 200-240 r/min at normal temperature for 20-30 min to obtain a polymer ethanol solution, adding the octylphenol polyoxyethylene ether and the sodium dodecyl sulfate into the deionized water, stirring at the rotating speed of 300-400 r/min under the water bath condition of 40-60 ℃ for 10-12 min, preserving heat to obtain an emulsifier solution, adding the modified heat storage and temperature regulation phase change microcapsules, the polymer ethanol solution and the hydroxypropyl silicone oil into the emulsifier, and (3) placing the mixture into a high-speed stirrer, stirring the mixture for 40-60 min at the rotating speed of 4000-6000 r/min under the water bath condition of 40-60 ℃, then placing the mixture into an ultrasonic dispersion machine, and ultrasonically dispersing the mixture for 20-30 min at the power of 400-500W at normal temperature to obtain the temperature-controlled finishing agent for the washable cotton fabric.

Example 1

Respectively weighing 20 parts by weight of n-octadecane, 12 parts by weight of acrylic acid, 40 parts by weight of ethyl acrylate, 24 parts by weight of vinyl acetate, 8 parts by weight of dodecyl trimethyl ammonium chloride, 0.4 part by weight of azobisisobutyronitrile and 120 parts by weight of deionized water, adding dodecyl trimethyl ammonium chloride into the deionized water, stirring at the rotating speed of 180r/min for 10min at normal temperature, dropwise adding 1% by weight of acetic acid to adjust the pH value to 5 to obtain a dodecyl trimethyl ammonium chloride mixed solution, adding the acrylic acid and the ethyl acrylate into the vinyl acetate, stirring and mixing at the rotating speed of 200r/min at normal temperature for 16min to obtain a mixed monomer, adding 1/2 parts by weight of the dodecyl trimethyl ammonium chloride mixed solution into the mixed monomer, placing the mixed monomer into a high-shear emulsifying machine, stirring and emulsifying at the rotating speed of 10000r/min at normal temperature for 1h to obtain a mixed emulsion, placing the n-octadecane into a, keeping the temperature to obtain n-octadecane liquid, adding azodiisobutyronitrile and the residual mixed solution of 1/2 mass dodecyl trimethyl ammonium chloride into the n-octadecane liquid, placing the n-octadecane liquid into a high-shear emulsifying machine, stirring and emulsifying the n-octadecane liquid for 30min at a rotation speed of 8000r/min under a water bath condition of 40 ℃, keeping the temperature to obtain n-octadecane mixed emulsion, slowly adding the mixed emulsion into the n-octadecane mixed emulsion at a dropping speed of 20mL/min, stirring the mixed emulsion for 1h at a rotation speed of 120r/min under a water bath condition of 70 ℃, keeping the temperature and standing the mixed solution for 4h to obtain microcapsule mixed solution, placing the microcapsule mixed solution into a centrifugal machine, centrifugally separating the microcapsule mixed solution for 20min at a rotation speed of 3000r/min at normal temperature, taking lower-layer solid, washing the mixture for 3 times by using deionized water, placing the washed mixture into an oven;

respectively weighing 20 parts of heat storage and temperature regulation phase change microcapsules, 4 parts of vinyltriethoxysilane, 2 parts of stearic acid and 120 parts of absolute ethyl alcohol, adding the vinyltriethoxysilane and the stearic acid into the absolute ethyl alcohol, stirring for 10min at the rotating speed of 260r/min under the water bath condition of 50 ℃, preserving heat to obtain a modified solution, adding the heat storage and temperature regulation phase change microcapsules into the modified solution, stirring for 30min at the rotating speed of 200r/min under the water bath condition of 40 ℃, placing the solution into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 20min at the normal temperature by the power of 500W to obtain a dispersion solution, placing the dispersion solution into a centrifugal machine, carrying out centrifugal separation for 10min at the rotating speed of 4000r/min at the normal temperature, taking lower-layer solids, washing for 3 times by the absolute ethyl alcohol, placing the mixture into a 60-DEG C oven to dry for 1h, and cooling at the normal temperature to obtain the modified heat storage and temperature regulation phase change;

respectively weighing 20 parts of modified heat storage temperature-regulating phase-change microcapsule, 16 parts of aqueous epoxy emulsion, 80 parts of absolute ethyl alcohol, 4 parts of polyethylene glycol, 10 parts of polyvinyl alcohol, 8 parts of hydroxypropyl silicone oil, 1 part of octylphenol polyoxyethylene ether, 0.8 part of sodium dodecyl sulfate and 20 parts of deionized water according to parts by weight, adding the aqueous epoxy emulsion, the polyethylene glycol and the polyvinyl alcohol into the absolute ethyl alcohol, stirring at the rotating speed of 200r/min for 20min at normal temperature to obtain polymer ethyl alcohol solution, adding the octylphenol polyoxyethylene ether and the sodium dodecyl sulfate into the deionized water, stirring at the rotating speed of 300r/min for 10min under the water bath condition of 40 ℃, preserving heat to obtain emulsifier solution, adding the modified heat storage temperature-regulating phase-change microcapsule, the polymer ethyl alcohol solution and the hydroxypropyl silicone oil into the emulsifier solution, placing in a high-speed stirrer, stirring at the rotating speed of 4000r/min for 40min under the water bath condition of 40 ℃, and placing the mixture in an ultrasonic dispersion machine, and ultrasonically dispersing the mixture for 20min at the normal temperature with the power of 400W to obtain the temperature-controlled finishing agent for the washable cotton fabric.

Example 2

Respectively weighing 30 parts by weight of n-octadecyl, 18 parts by weight of acrylic acid, 60 parts by weight of ethyl acrylate, 36 parts by weight of vinyl acetate, 12 parts by weight of dodecyl trimethyl ammonium chloride, 0.6 part by weight of azobisisobutyronitrile and 180 parts by weight of deionized water, adding dodecyl trimethyl ammonium chloride into the deionized water, stirring at the rotation speed of 190r/min for 11min at normal temperature, dropwise adding 1% by weight of acetic acid to adjust the pH to 5.5 to obtain a dodecyl trimethyl ammonium chloride mixed solution, adding the acrylic acid and the ethyl acrylate into the vinyl acetate, stirring and mixing at the rotation speed of 220r/min at normal temperature for 18min to obtain a mixed monomer, adding 1/2 parts by weight of the dodecyl trimethyl ammonium chloride mixed solution into the mixed monomer, placing the mixed monomer into a high-shear emulsifying machine, stirring and emulsifying at the rotation speed of 12000r/min at normal temperature for 1.5h to obtain a mixed emulsion, placing the n-octadecyl under the water bath condition, keeping the temperature to obtain n-octadecane liquid, adding azodiisobutyronitrile and the residual mixed solution of 1/2 mass dodecyl trimethyl ammonium chloride into the n-octadecane liquid, placing the n-octadecane liquid into a high-shear emulsifying machine, stirring and emulsifying the n-octadecane liquid at a rotating speed of 9000r/min under a water bath condition of 50 ℃, keeping the temperature to obtain n-octadecane mixed emulsion, slowly adding the mixed emulsion into the n-octadecane mixed emulsion at a dropping speed of 25mL/min, stirring the mixed emulsion at a rotating speed of 140r/min under a water bath condition of 75 ℃, keeping the temperature and standing for 5 hours to obtain microcapsule mixed liquid, placing the microcapsule mixed liquid into a centrifugal machine, centrifugally separating the microcapsule mixed liquid at a rotating speed of 3250r/min for 25 minutes at normal temperature, taking lower-layer solid, washing the lower-layer solid with deionized water for 4 times, placing the washed solid in a baking oven, and drying the mixture for 25 minutes at;

respectively weighing 30 parts of heat storage and temperature regulation phase change microcapsules, 6 parts of vinyltriethoxysilane, 3 parts of stearic acid and 180 parts of absolute ethyl alcohol, adding the vinyltriethoxysilane and the stearic acid into the absolute ethyl alcohol, stirring for 15min at a rotation speed of 270r/min under a water bath condition of 55 ℃, preserving heat to obtain a modified solution, adding the heat storage and temperature regulation phase change microcapsules into the modified solution, stirring for 35min at a rotation speed of 220r/min under a water bath condition of 45 ℃, placing the solution into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 25min at normal temperature with a power of 550W to obtain a dispersion solution, placing the dispersion solution into a centrifugal machine, carrying out centrifugal separation for 15min at a rotation speed of 4500r/min at normal temperature, taking a lower layer of solid, washing for 4 times with the absolute ethyl alcohol, drying for 1.5h in an oven at 70 ℃, and cooling at normal temperature to obtain the modified heat storage and temperature regulation phase change microcapsules;

respectively weighing 30 parts of modified heat storage temperature-regulating phase-change microcapsule, 24 parts of aqueous epoxy emulsion, 120 parts of absolute ethyl alcohol, 6 parts of polyethylene glycol, 15 parts of polyvinyl alcohol, 12 parts of hydroxypropyl silicone oil, 1.5 parts of octyl phenol polyoxyethylene ether, 1.2 parts of lauryl sodium sulfate and 30 parts of deionized water according to parts by weight, adding the aqueous epoxy emulsion, the polyethylene glycol and the polyvinyl alcohol into the absolute ethyl alcohol, stirring for 25min at the rotating speed of 220r/min at normal temperature to obtain polymer ethanol solution, adding the octyl phenol polyoxyethylene ether and the lauryl sodium sulfate into the deionized water, stirring for 11min at the rotating speed of 350r/min under the water bath condition of 50 ℃, preserving heat to obtain emulsifier solution, adding the modified heat storage temperature-regulating phase-change microcapsule, the polymer ethanol solution and the hydroxypropyl silicone oil into the emulsifier solution, placing the emulsifier solution in a high-speed stirrer, stirring for 50min at the rotating speed of 5000r/min under the water bath condition of 50 ℃, and then placing the mixture into an ultrasonic dispersion machine, and ultrasonically dispersing the mixture for 25min at normal temperature with the power of 450W to obtain the temperature-controlled finishing agent for the washable cotton fabric.

Example 3

Respectively weighing 40 parts by weight of n-octadecane, 24 parts by weight of acrylic acid, 80 parts by weight of ethyl acrylate, 48 parts by weight of vinyl acetate, 16 parts by weight of dodecyl trimethyl ammonium chloride, 0.8 part by weight of azobisisobutyronitrile and 240 parts by weight of deionized water, adding dodecyl trimethyl ammonium chloride into the deionized water, stirring at the rotating speed of 200r/min for 12min at normal temperature, dropwise adding 1% by weight of acetic acid to adjust the pH value to 6 to obtain a dodecyl trimethyl ammonium chloride mixed solution, adding the acrylic acid and the ethyl acrylate into the vinyl acetate, stirring and mixing at the rotating speed of 240r/min at normal temperature for 20min to obtain a mixed monomer, adding 1/2 parts by weight of the dodecyl trimethyl ammonium chloride mixed solution into the mixed monomer, placing the mixed monomer into a high-shear emulsifying machine, stirring and emulsifying at the rotating speed of 14000r/min at normal temperature for 2h to obtain a mixed emulsion, placing the n-octadecane into a, keeping the temperature to obtain n-octadecane liquid, adding azodiisobutyronitrile and the residual mixed solution of 1/2 mass dodecyl trimethyl ammonium chloride into the n-octadecane liquid, placing the n-octadecane liquid into a high-shear emulsifying machine, stirring and emulsifying the n-octadecane liquid for 40min at 10000r/min under the condition of 60 ℃ water bath, keeping the temperature to obtain n-octadecane mixed emulsion, slowly adding the mixed emulsion into the n-octadecane mixed emulsion at the dropping speed of 30mL/min, stirring the mixed emulsion for 2h at 160r/min under the condition of 80 ℃ water bath, keeping the temperature and standing for 6h to obtain microcapsule mixed liquid, placing the microcapsule mixed liquid into a centrifugal machine, centrifugally separating the microcapsule mixed liquid for 30min at 3500r/min at normal temperature, taking lower-layer solid, washing the lower-layer solid for 5 times by using deionized water, placing the washed solid into an oven, and drying the mixture for 30min at 60 ℃;

respectively weighing 40 parts of heat storage and temperature regulation phase change microcapsules, 8 parts of vinyltriethoxysilane, 4 parts of stearic acid and 240 parts of absolute ethyl alcohol, adding the vinyltriethoxysilane and the stearic acid into the absolute ethyl alcohol, stirring for 20min at the rotating speed of 280r/min under the water bath condition of 60 ℃, preserving heat to obtain a modified solution, adding the heat storage and temperature regulation phase change microcapsules into the modified solution, stirring for 40min at the rotating speed of 240r/min under the water bath condition of 50 ℃, placing the solution into an ultrasonic dispersion machine, carrying out ultrasonic treatment for 30min at normal temperature with the power of 600W to obtain a dispersion solution, placing the dispersion solution into a centrifugal machine, carrying out centrifugal separation for 20min at the rotating speed of 5000r/min at normal temperature, taking lower-layer solids, washing for 5 times with the absolute ethyl alcohol, placing the mixture into an oven at 80 ℃ for drying for 2h, and cooling at normal temperature to obtain the modified heat storage and temperature regulation phase change microcapsules;

respectively weighing 40 parts of modified heat storage temperature-regulating phase-change microcapsule, 32 parts of aqueous epoxy emulsion, 160 parts of absolute ethyl alcohol, 8 parts of polyethylene glycol, 20 parts of polyvinyl alcohol, 16 parts of hydroxypropyl silicone oil, 2 parts of octylphenol polyoxyethylene ether, 1.6 parts of sodium dodecyl sulfate and 40 parts of deionized water according to parts by weight, adding the aqueous epoxy emulsion, the polyethylene glycol and the polyvinyl alcohol into the absolute ethyl alcohol, stirring at 240r/min for 30min at normal temperature to obtain polymer ethanol solution, adding the octylphenol polyoxyethylene ether and the sodium dodecyl sulfate into the deionized water, stirring at 400r/min for 12min under the water bath condition of 60 ℃, preserving heat to obtain emulsifier solution, adding the modified heat storage temperature-regulating phase-change microcapsule, the polymer ethanol solution and the hydroxypropyl silicone oil into the emulsifier solution, placing in a high-speed stirrer, stirring at 6000r/min for 60min under the water bath condition of 60 ℃, and then placing the mixture into an ultrasonic dispersion machine, and ultrasonically dispersing the mixture for 30min at the normal temperature with the power of 500W to obtain the temperature-controlled finishing agent for the washable cotton fabric.

Comparative example: temperature regulating textile manufactured by Dongguan company.

The temperature-adjusting textiles prepared in the examples and the comparative examples are detected, and the specific detection is as follows:

air permeability: the air permeability of the textile fabric is measured according to GB/T5453-2009 permeability test method for textile fabrics.

Washing weight loss rate of fabric: the weights m1 (g) and m2 (g) of the fabric before and after washing were weighed with an electronic balance and calculated using the formula.

The fabric temperature adjusting performance is as follows: the self-made temperature-regulating textile tester simulates the blood circulation of a human body by using circulating water, keeps the water temperature at 30 ℃ unchanged, respectively wraps unfinished and finished textiles by two temperature sensors, regulates the temperature change range by a heating source at 10-40 ℃, and records the temperature change.

The specific test results are shown in table 1.

Table 1 comparative table of property characterization

Detecting items	Example 1	Example 2	Example 3	Comparative example
					Air permeability/mm/s	3.6	3.8	3.7	2.5
Water washing weight loss rate/%)	13	15	14	23
					Temperature control Performance/. degree.C.m-2·min-1	600～700	600～700	600～700	520～810

As can be seen from Table 1, the temperature-controlled finishing agent for the washable cotton fabric prepared by the invention has good washing resistance and temperature regulation capability.