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CN-122013509-A - Preparation method of intelligent temperature control textile based on phase change microcapsules

CN122013509ACN 122013509 ACN122013509 ACN 122013509ACN-122013509-A

Abstract

The invention relates to the technical field of non-woven materials and engineering, in particular to a preparation method of an intelligent temperature-controlled textile based on phase-change microcapsules, which comprises the following steps of adding polyurethane prepolymer and composite phase-change material into a three-neck flask, heating to 80-100 ℃ to enable all components to be in a molten state, then putting the mixture into a high-speed shearing emulsifying machine, slowly increasing the rotating speed to 8000-9000 r/min, slowly adding a certain amount of deionized water containing 1-2 g/L defoamer DM8317 into 30-40 min, stirring for 60-120 min, after obtaining uniform emulsion, reducing the rotating speed to 400-450 r/min, adding 1-2g of initiator potassium persulfate, heating to 50-70 ℃ to react for 3-4 h. Graphene is added to the core material and the wall material, so that the temperature adjustment rate is increased.

Inventors

  • QI MING
  • LI YIMIN
  • WU LIANGHUA
  • WANG YANQING
  • LI YIFENG
  • WEI BINGJU

Assignees

  • 浙江森马服饰股份有限公司
  • 浙江三元纺织有限公司

Dates

Publication Date
20260512
Application Date
20260313

Claims (10)

  1. 1. The preparation method of the intelligent temperature control textile based on the phase change microcapsule is characterized by comprising the following steps of: (1) Preparation of aqueous phase-change microcapsule emulsion Adding polyurethane prepolymer and composite phase change material into a three-neck flask, heating to 80-100 ℃ to enable all components to be in a molten state, then putting the mixture into a high-speed shearing emulsifying machine, slowly increasing the rotating speed to 8000-9000 r/min, slowly adding a certain amount of deionized water containing 1-2 g/L defoamer DM8317 within 30-40 min, stirring for 60-120 min to obtain uniform emulsion, reducing the rotating speed to 400-450 r/min, adding 1-2g of initiator potassium persulfate, heating to 50-70 ℃ to react for 3-4 h, cooling to room temperature, and removing acetone by rotary evaporation to obtain aqueous phase change microcapsule emulsion; Wherein the polyurethane prepolymer is prepared by the following steps Placing polyglycol into a three-neck flask, heating the polyglycol to a molten state in a constant-temperature blast drying oven at 115-125 ℃, cooling to 50-60 ℃, adding isocyanate, heating to 60-70 ℃ for reaction for 60-70 min, then adding 0.6-1 mL dibutyl tin dilaurate, heating to 70-80 ℃ in a reflux state, continuing to react for 60-90 min, then adding modified graphene A, dimethylolpropionic acid, hydroxyethyl acrylate, epoxy resin and 20-30 g of acetone, heating to 80-90 ℃, reacting at a constant temperature for 60-90 min, and cooling to 30-35 ℃ to obtain polyurethane prepolymer; In the preparation method of the polyurethane prepolymer, the epoxy resin is one or more of EP-12, EP-13, EP-16 and EP-20, and the mass ratio of diisocyanate, polyglycol, modified graphene, dimethylolpropionic acid, hydroxyethyl acrylate and epoxy resin is 25:30:3:10:8:5; Dispersing 5-10 g of graphene in 500-550 mL of deionized water by ultrasonic, adding 50-80 g of methoxytrimethylsilane, adjusting the rotating speed of a stirrer to 300-400 r/min, reacting at 30-40 ℃ for 60-120 min, heating to 40-60 ℃ for 30-60 min, adding 10-20 g of 3-glycidoxypropyl trimethoxysilane, continuously reacting for 30-60 min, fully washing with deionized water, and drying; wherein the composite phase change material is prepared by the following steps Placing 100-110 g of paraffin into a round-bottom flask, heating to 80-100 ℃ to enable the paraffin to be in a molten state, adding 0.3-0.5 g of modified graphene B, and uniformly mixing under stirring at 500-550 r/min; the preparation method of the modified graphene B comprises the following steps of dispersing 5-10 g of graphene in 500-550 mL of deionized water in an ultrasonic manner, adding 80-120 g of methoxytrimethylsilane, adjusting the rotating speed of a stirrer to 300-400 r/min, reacting for 60-120 min at 30-40 ℃, heating to 40-60 ℃ and reacting for 60-90 min, fully washing with deionized water, and drying; (2) Preparation of intelligent temperature-controlled textile of phase-change microcapsule And (3) finishing the aqueous phase-change microcapsule emulsion prepared in the step (1) into textiles by adopting a two-soaking and two-rolling method, wherein the rolling surplus rate is 60-65%, pre-baking for 2-5min at 80-90 ℃ and then baking for 3-5min at 140-160 ℃, and the concentration of the aqueous phase-change microcapsule emulsion is 60-100 g/L.
  2. 2. The method for preparing the intelligent temperature-controlled textile based on the phase-change microcapsule according to claim 1, wherein the mass ratio of the polyurethane prepolymer to the composite phase-change material is 1:1.
  3. 3. The method for preparing the intelligent temperature-controlled textile based on the phase-change microcapsule according to claim 1, wherein the solid content of the aqueous phase-change microcapsule emulsion is 25%.
  4. 4. The method for preparing the intelligent temperature-controlled textile based on the phase-change microcapsules according to claim 1, wherein the polyglycol is any one of polycaprolactone glycol PCL, polyether glycol PPG and polytetrahydrofuran glycol PTMEG.
  5. 5. The method for preparing the intelligent temperature-controlled textile based on the phase-change microcapsules according to claim 1, wherein the diisocyanate is one or a mixture of hexamethylene diisocyanate, diphenylmethane diisocyanate, pentamethylene diisocyanate, 4 '-dicyclohexylmethane diisocyanate and triphenylmethane triisocyanate, and the compound molar ratio of hexamethylene diisocyanate, 4' -dicyclohexylmethane diisocyanate and triphenylmethane triisocyanate is 3:6:1.
  6. 6. The preparation method of the intelligent temperature-controlled textile based on the phase-change microcapsules, which is disclosed in claim 1, is characterized in that in the preparation method of the modified graphene A, the mass ratio of the graphene, the methoxytrimethylsilane and the 3-glycidoxypropyl trimethoxysilane is 1:6:1.5.
  7. 7. The method for preparing the intelligent temperature-controlled textile based on the phase-change microcapsules, which is characterized in that the textile is made of one or more of natural cellulose fibers, regenerated fiber fibers, polyamide fibers and polyester fibers.
  8. 8. The method for preparing intelligent temperature-controlled textile based on phase-change microcapsules according to claim 1, wherein the textile is one of a woven textile, a knitted textile and a non-woven textile.
  9. 9. The preparation method of the intelligent temperature-controlled textile based on the phase-change microcapsules is characterized in that the high-speed shearing emulsifying machine comprises a base bracket (3), rollers (2) for realizing the integral movement of equipment are arranged around the bottom of the base bracket (3), a lifting bracket (7) is vertically arranged on one side of the base bracket (3), a plurality of guide rods (16) are arranged between the top and the bottom of the inner wall of the lifting bracket (7) and are correspondingly arranged, a motor mounting plate (12) is arranged at one end of the top of the guide rod (16) and a sliding guide sleeve (17) is arranged at the joint of the guide rods, a shearing emulsifying mechanism is connected to one end of the motor mounting plate (12), the shearing emulsifying mechanism comprises a driving motor (11), an output shaft (9) is connected to one end of the bottom of the driving motor (11), a plurality of positioning rods (10) are arranged around the output shaft (9) at equal intervals, stirring heads are jointly arranged at the bottoms of the output shaft (9) and the positioning rods (10), an emulsifying container (4) is arranged at the bottom of the stirring heads, a plurality of supporting legs (1) are arranged at the bottoms of the emulsifying container (4), a driving component (15) is arranged on one side of the base bracket (3), a vertical driving component (15) is arranged on one side, a lifting component (15) is arranged on the lifting component and comprises a lifting component for fixing the lifting component, the fixed base (15) is associated with the base support (3), a hydraulic oil cylinder (14) is arranged at the top of the fixed base (15), one end of the hydraulic oil cylinder (14) is connected with a piston rod (13), and one end of the piston rod (13) is associated with the bottom of the motor mounting plate (12).
  10. 10. The preparation method of the intelligent temperature control textile based on the phase-change microcapsules is characterized in that the protective baffle assembly comprises anti-splashing baffles (6), the anti-splashing baffles (6) are bent towards the emulsifying container (4) to form bending parts (5), an observation window (8) is arranged in the center of the outer wall of each anti-splashing baffle (6), LED lamp groups (18) are arranged in the center of the inner wall of each bending part (5) of each anti-splashing baffle (6), and the number of the LED lamp groups (18) is 20-30 and the LED lamp groups are arranged in an equidistant array.

Description

Preparation method of intelligent temperature control textile based on phase change microcapsules Technical Field The invention relates to the technical field of non-woven materials and engineering, in particular to a preparation method of an intelligent temperature control textile based on phase-change microcapsules. Background The traditional textile mostly adopts the change of fabric structure or fiber variety to reduce the serious influence of temperature change on the physical and mental health of human body, but the comfort and the functionality cannot be considered. The phase-change intelligent temperature-control textile can utilize the phase-change material to absorb or release a large amount of heat in the phase-change process, keep the temperature in microclimate of human body and clothing basically constant within a certain time, can effectively prevent heat stress reaction, and can meet the requirement of human body comfort under extreme environmental conditions. At present, the preparation method of the phase-change intelligent temperature-control textile mainly comprises three methods of a hollow fiber dipping filling method, a spinning method and a post-finishing method. The hollow fiber impregnation method is a temperature-regulating fiber preparation method for adsorbing and storing phase-change materials by utilizing the inside of pore channels of the hollow fibers, but the phase-change materials are easy to migrate out of the fibers after the temperature-regulating textile prepared by the method is subjected to a plurality of phase-transition processes, so that the service performance of the temperature-regulating textile is severely limited. The spinning method refers to suspending phase-change microcapsules in a spinning solution and forming fibers through spinning (such as electrostatic spinning, wet spinning, melt spinning and the like), or mixing encapsulated phase-change materials with other types of fibers and spinning into textiles. The post-finishing method is to adhere the phase change material in the form of finishing liquid temporarily or permanently in the fabric in the form of dipping, padding, coating and the like, and has the advantages of simple operation, relatively low cost, wide applicability to fibers and the like, but the adhesive used in the method can reduce the softness, flexibility, air permeability and moisture permeability of the fabric, and finally affect the wearing comfort. In order to solve the problem of adhesives, CN116024821A discloses a finishing method of textiles with phase-change microcapsules, the shell material of the phase-change microcapsules prepared by the method is diacetone acrylamide-adipic dihydrazide self-crosslinking resin, in the drying process, active ketone carbonyl in the shell material reacts with active alpha-H in adipic dihydrazide under the weak acid condition, so that the crosslinking reaction is gradually completed, the self-crosslinking among microcapsule particles forms a film, and finally the film is stably adsorbed on the surface or pores of the textiles. The microcapsules prepared by the method form a film through self-crosslinking, so that the effect of improving the binding force between the microcapsules and the fibers is poor, and the improvement degree of effect durability is limited. At present, the phase change materials mainly comprise organic, inorganic and composite phase change materials, wherein the organic phase change materials have the characteristics of various types, no toxicity, no supercooling and the like, and are the most studied phase change materials. The paraffin has no functional group and free movable electrons, so that the paraffin has higher chemical stability, does not cause chemical reaction or damage other materials in the phase change process, and the chemical inertness and the characteristic of high heat storage density of the paraffin enable the paraffin to store a large amount of heat energy in a relatively small volume, so that the paraffin has become one of important points in the field of phase change material research. It is well known that thermal conductivity is a major factor in enhancing the rate of heat transfer, playing an important role in the melting and solidification process. However, the irregular crystal structure makes the paraffin slower in heat transfer upon energy storage and release, resulting in a significant decrease in thermal performance of the heat storage system. Aiming at the problem of low thermal conductivity of the paraffin phase-change material, researchers improve the thermal characteristics of the phase-change material by compounding paraffin with other materials, adding metal nano particles and the like. Researches show that graphene is the best material for improving the thermal conductivity of paraffin, but the surface of unmodified graphene contains a large number of hydrophilic groups such as carboxyl, hydroxyl and epoxy groups, so that the uniform d