CN113604896A - Energy-storage temperature-regulating lyocell fiber and preparation method thereof - Google Patents
Energy-storage temperature-regulating lyocell fiber and preparation method thereof Download PDFInfo
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- CN113604896A CN113604896A CN202110911718.6A CN202110911718A CN113604896A CN 113604896 A CN113604896 A CN 113604896A CN 202110911718 A CN202110911718 A CN 202110911718A CN 113604896 A CN113604896 A CN 113604896A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
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Abstract
The invention belongs to the technical field of cellulose fibers, and particularly relates to an energy-storing and temperature-adjusting lyocell fiber and a preparation method thereof. The invention provides energy-storage and temperature-regulation lyocell fiber which comprises lyocell fiber and energy-storage and temperature-regulation microcapsules crosslinked with the lyocell fiber, wherein each energy-storage and temperature-regulation microcapsule comprises a capsule wall and a capsule core, each capsule core comprises a phase-change material and a nano nucleating agent, and each capsule wall comprises melamine modified urea-formaldehyde resin prepolymer. The energy storage and temperature regulation microcapsules in the energy storage and temperature regulation lyocell fibers are crosslinked with the lyocell fiber matrix, so that the stability of the energy storage and temperature regulation microcapsules in the energy storage and temperature regulation lyocell fibers is improved, the loss of the energy storage and temperature regulation microcapsules in the use process of the fibers is reduced, and the functionality of the energy storage and temperature regulation lyocell fibers is prolonged.
Description
Technical Field
The invention belongs to the technical field of cellulose fibers, and particularly relates to an energy-storing and temperature-adjusting lyocell fiber and a preparation method thereof.
Background
With the development of science and technology and the improvement of the living standard of people, the fiber industry gradually develops towards functionalization and intellectualization, and the energy storage and temperature adjustment fiber is an important fiber. The energy storage temperature regulating fiber has a bidirectional automatic temperature regulating function, and the purpose of regulating the temperature is achieved by utilizing latent heat released or absorbed by the phase change material in the phase change process.
Most of the existing energy storage and temperature regulation fibers are based on viscose fibers, and for example, the researches on the temperature regulation and modification of the viscose fibers are disclosed in Chinese patents ZL200610157441.8, ZL200710014607.5, ZL200710123411.X, ZL201010164832.9, ZL201010295055.1, ZL201210357126.5, ZL201310420382.9 and ZL201410616024. X. However, the viscose fiber spinning process is long in flow, and chemical raw materials such as sodium hydroxide, carbon disulfide and sulfuric acid are used in the production process, so that the pollution is serious. Accordingly, the energy storage and temperature regulation fiber using the lyocell fiber as the matrix is produced.
The lyocell fiber is a regenerated cellulose fiber prepared by using N-methylmorpholine-N-oxide (NMMO) as a direct cellulose solvent through a dry-jet wet spinning process. Compared with viscose fiber, the lyocell fiber has the advantages of simple and green production process, especially physical and mechanical properties, good dimensional stability and high favor of consumers. Chinese patent CN201911301213.7 discloses a temperature-adjusting lyocell fiber and a preparation method thereof. According to the patent technology, the semi-refined paraffin mixture is directly added into spinning slurry of the lyocell fiber as a phase-change material for realizing the temperature regulation function, so that the lyocell fiber with the energy storage and temperature regulation functions is prepared. However, the phase change material in the lyocell fiber with the energy storage and temperature regulation functions disclosed in the patent is easy to run off, and the service life of the fiber in energy storage and temperature regulation is influenced.
Disclosure of Invention
In view of the above, the invention provides an energy storage and temperature regulation lyocell fiber and a preparation method thereof, wherein the energy storage and temperature regulation microcapsules in the energy storage and temperature regulation lyocell fiber are crosslinked with the lyocell fiber, so that the stability of the energy storage and temperature regulation microcapsules in the energy storage and temperature regulation lyocell fiber is improved, and the long-term maintenance of the functionality of the energy storage and temperature regulation lyocell fiber is facilitated.
In order to solve the technical problem, the invention provides energy-storage temperature-regulating lyocell fiber which comprises lyocell fiber and energy-storage temperature-regulating microcapsules crosslinked with the lyocell fiber, wherein each energy-storage temperature-regulating microcapsule comprises a capsule wall and a capsule core, each capsule core comprises a phase-change material and a nano nucleating agent, and each capsule wall comprises melamine modified urea-formaldehyde resin prepolymer.
Preferably, the mass ratio of the lyocell fibers to the energy-storage temperature-regulating microcapsules is 100: 17.5 to 49.0.
Preferably, the capsule wall further comprises nano zinc oxide.
Preferably, the phase change material comprises paraffin, n-octadecane, n-nonadecane or n-eicosane;
the nano nucleating agent comprises nano zinc oxide, nano titanium dioxide, nano calcium carbonate or nano silicon dioxide; the grain size of the nano nucleating agent is 15-50 nm;
the mass ratio of the nano nucleating agent to the phase-change material is 0.2-0.3: 10.
Preferably, the mass ratio of the nano zinc oxide to the melamine modified urea-formaldehyde resin prepolymer is 0.1-0.3: 1.
The invention also provides a preparation method of the energy-storage temperature-regulating lyocell fiber, which comprises the following steps:
mixing the energy-storage temperature-regulating microcapsule, the cellulose pulp and the N-methylmorpholine-N-oxide aqueous solution, and then carrying out post-treatment to obtain a spinning stock solution;
and carrying out microwave treatment on the spinning stock solution after spinning to obtain the energy-storage temperature-regulating lyocell fiber.
Preferably, the microwave frequency of the microwave treatment is 1560-1800 MHz, and the time is 20-36 min.
Preferably, the mass percentage of the alpha cellulose in the cellulose pulp is 92-99%, and the mass ratio of the energy storage and temperature regulation microcapsule to the cellulose pulp is 18-50: 100.
Preferably, the preparation method of the energy storage and temperature regulation microcapsule comprises the following steps:
firstly mixing the phase change material, the nano nucleating agent, the emulsifier and water to obtain capsule core material emulsion;
mixing glutaraldehyde, formaldehyde, melamine, urea and water for a second time, and carrying out polycondensation reaction to obtain a melamine modified urea-formaldehyde resin prepolymer;
and thirdly, mixing the melamine modified urea-formaldehyde resin prepolymer, the nano zinc oxide and the capsule core material emulsion for carrying out capsule wall crosslinking reaction to obtain the energy-storage temperature-regulating microcapsule.
Preferably, the temperature of the polycondensation reaction is 40-50 ℃;
the temperature of the capsule wall crosslinking reaction is 65-75 ℃; the time is 150-240 min.
The invention provides energy-storage and temperature-regulation lyocell fiber which comprises lyocell fiber and energy-storage and temperature-regulation microcapsules crosslinked with the lyocell fiber, wherein each energy-storage and temperature-regulation microcapsule comprises a capsule wall and a capsule core, each capsule core comprises a phase-change material and a nano nucleating agent, and each capsule wall comprises melamine modified urea-formaldehyde resin prepolymer. In the invention, the hydroxymethyl in the melamine modified urea-formaldehyde resin prepolymer and the hydroxyl in the lyocell fiber are subjected to polycondensation reaction, so that the stability of the energy storage and temperature regulation microcapsule is improved; meanwhile, the amino group in the melamine modified urea resin prepolymer can form a hydrogen bond with the hydroxyl group in the lyocell fiber, so that the stability of the energy storage and temperature regulation microcapsule is further improved, the loss of the energy storage and temperature regulation microcapsule in the use process of the energy storage and temperature regulation lyocell fiber is reduced, and the functionality of the energy storage and temperature regulation lyocell fiber is prolonged.
The invention also provides a preparation method of the energy-storage temperature-regulating lyocell fiber, which comprises the following steps: mixing the energy-storage temperature-regulating microcapsule, the cellulose pulp and the N-methylmorpholine-N-oxide aqueous solution, and then carrying out post-treatment to obtain a spinning stock solution; and carrying out microwave treatment on the spinning stock solution after spinning to obtain the energy-storage temperature-regulating lyocell fiber. The preparation method provided by the invention has the advantages of short production process flow, no need of adding strong base or strong acid in the production process, greenness and no pollution.
Detailed Description
The invention provides energy-storage and temperature-regulation lyocell fiber which comprises lyocell fiber and energy-storage and temperature-regulation microcapsules crosslinked with the lyocell fiber, wherein each energy-storage and temperature-regulation microcapsule comprises a capsule wall and a capsule core, each capsule core comprises a phase-change material and a nano nucleating agent, and each capsule wall comprises melamine modified urea-formaldehyde resin prepolymer.
In the invention, the capsule core of the energy-storing and temperature-adjusting microcapsule comprises a phase-change material and a nano nucleating agent; the phase change material preferably comprises paraffin, n-octadecane, n-nonadecane or n-eicosane, more preferably n-octadecane or n-eicosane. In the present invention, the nano nucleating agent preferably comprises nano zinc oxide, nano titanium dioxide, nano calcium carbonate or nano silicon dioxide, more preferably nano zinc oxide; the particle size of the nano nucleating agent is preferably 15-50 nm, and more preferably 25-38 nm. In the invention, the mass ratio of the nano nucleating agent to the phase-change material is preferably 0.2-0.3: 10, more preferably 0.25-0.28: 10. in the invention, the nano nucleating agent serving as a crystal nucleus can promote crystallization, reduce supercooling degree in the phase change process and improve the energy storage and temperature regulation efficiency of the phase change material.
In the invention, the capsule wall of the energy-storage temperature-regulating microcapsule comprises melamine modified urea-formaldehyde resin prepolymer, and preferably also comprises nano zinc oxide. In the invention, the particle size of the nano zinc oxide is preferably 15-50 nm, and more preferably 20-35 nm. In the invention, the nano zinc oxide in the capsule wall endows the energy-storing and temperature-adjusting lyocell fiber with an antibacterial function.
In the invention, the mass ratio of the nano zinc oxide to the melamine modified urea resin prepolymer is preferably 0.1-0.3: 1, and more preferably 0.16-0.25: 1.
In the present invention, the preparation method of the melamine modified urea resin prepolymer preferably comprises the following steps: mixing glutaraldehyde, formaldehyde, melamine, urea and water for polycondensation reaction to obtain the melamine modified urea-formaldehyde resin prepolymer. In the present invention, the formaldehyde is preferably provided in the form of an aqueous formaldehyde solution; in the present invention, the mass concentration of the formalin is preferably 35 to 39%, and more preferably 37%. In the invention, the mass ratio of the glutaraldehyde to the formaldehyde is preferably 1: 1-3, and more preferably 1: 1.8-2.5; the mass ratio of the melamine to the urea is preferably 0.05-0.15: 1, and more preferably 0.08-0.12: 1. In the invention, the ratio of the total mass of glutaraldehyde and formaldehyde to the total mass of melamine and urea is preferably 2-4: 1, and more preferably 2.5-3: 1. The mixing is not particularly limited as long as the uniform mixing can be achieved. In the present invention, it is preferable to further include, before the polycondensation reaction: and adjusting the pH value of the mixed product to 7.5-8.5, and preferably 8. In the present invention, the pH adjusting agent for adjusting pH preferably includes triethanolamine or sodium hydroxide, more preferably triethanolamine. The invention has no special requirement on the dosage of the pH value regulator, as long as the pH value can be regulated to the required pH value. In the present invention, the polycondensation reaction is preferably accompanied by stirring, and the rotation speed of the stirring is preferably 200 to 400r/min, more preferably 260 to 320 r/min. In the invention, the temperature of the polycondensation reaction is preferably 60-90 ℃, and more preferably 70-80 ℃. In the present invention, the time of the polycondensation reaction is not particularly limited as long as the reaction system is formed into a colorless transparent solution.
In the present invention, the mass ratio of the lyocell fibers to the energy storage and temperature regulation microcapsules is preferably 100: 17.5 to 49.0, more preferably 100: 27.3 to 37.1.
The invention also provides a preparation method of the energy-storage temperature-regulating lyocell fiber, which comprises the following steps:
mixing the energy-storage temperature-regulating microcapsule, the cellulose pulp and the N-methylmorpholine-N-oxide aqueous solution, and then carrying out post-treatment to obtain a spinning stock solution;
and carrying out microwave treatment on the spinning stock solution after spinning to obtain the energy-storage temperature-regulating lyocell fiber.
The invention mixes the energy-storing temperature-adjusting microcapsule, cellulose pulp and N-methylmorpholine-N-oxide aqueous solution and carries out post-treatment to obtain spinning solution. In the present invention, the preparation method of the energy storage and temperature regulation microcapsule preferably comprises the following steps:
firstly mixing the phase change material, the nano nucleating agent, the emulsifier and water to obtain capsule core material emulsion;
mixing glutaraldehyde, formaldehyde, melamine, urea and water for a second time, and carrying out polycondensation reaction to obtain a melamine modified urea-formaldehyde resin prepolymer;
and thirdly, mixing the melamine modified urea-formaldehyde resin prepolymer, the nano zinc oxide and the capsule core material emulsion for carrying out capsule wall crosslinking reaction to obtain the energy-storage temperature-regulating microcapsule.
The invention mixes the phase-change material, the nano nucleating agent, the emulsifier and the water for the first time to obtain the capsule core material emulsion. In the present invention, the first mixing preferably includes the steps of:
melting the phase-change material, and mixing with the nano nucleating agent to obtain a capsule core material;
dispersing an emulsifier in water to obtain an emulsifier dispersion;
and fifthly, mixing the capsule core material and the emulsion dispersion liquid to obtain the capsule core material emulsion liquid.
The phase-change material is melted and then mixed with the nano nucleating agent to obtain the capsule core material. In the present invention, the phase change material preferably includes paraffin, n-octadecane, n-nonadecane or n-eicosane, more preferably n-octadecane or n-eicosane. In the present invention, the nano nucleating agent preferably comprises nano zinc oxide, nano titanium dioxide, nano calcium carbonate or nano silica, more preferably nano zinc oxide. In the invention, the particle size of the nano nucleating agent is preferably 15-50 nm, and more preferably 25-38 nm. In the invention, the mass ratio of the nano nucleating agent to the phase change material is preferably 0.2-0.3: 10, and more preferably 0.25-0.28: 10.
In the invention, the melting temperature is preferably 40-50 ℃, and more preferably 42-48 ℃. In the present invention, the time for melting is not particularly limited as long as the phase change material can be melted. In the invention, the fourth mixing is preferably carried out under the condition of stirring, and the rotating speed of the stirring is preferably 600-850 r/min, and more preferably 680-800 r/min. The stirring time is not particularly limited, and the stirring time is not particularly limited as long as the stirring time can be uniformly mixed.
The invention disperses the emulsifier in water to obtain the emulsifier dispersion. In the present invention, the emulsifier preferably includes one or more of tween-80, Sodium Dodecyl Sulfate (SDS), span-80 and styrene maleic anhydride sodium salt, more preferably tween-80 or span-80. When the emulsifier comprises more than two specific substances, the mass ratio of the specific substances is not particularly limited, and any ratio can be adopted. In the present invention, the water is preferably distilled water. The dispersion is not particularly limited in the present invention as long as the dispersion can be uniformly dispersed.
After the capsule core material and the emulsion dispersion liquid are obtained, the capsule core material and the emulsion dispersion liquid are mixed for the fifth time to obtain the capsule core material emulsion liquid. In the invention, the mass percentage of the capsule core material in the capsule core material emulsion is preferably 30-40%, and more preferably 32.5-36.8%; the mass percentage of the emulsifier in the capsule core material emulsion is 2.5-4%, and the preferable mass percentage is 3.2-3.75%. In the invention, the temperature of the fifth mixing is preferably 40-50 ℃, and more preferably 42-46 ℃; the fifth mixing is preferably carried out under the condition of stirring, and the rotating speed of the stirring is preferably 1800-2300 r/min, and more preferably 1980-2150 r/min. The particle size of the emulsion droplets is preferably detected in the fifth mixing process, and the particle size is preferably D90 ≦ 1.055 μm, more preferably 0.892 μm ≦ D90 ≦ 0.998 μm. The stirring time is not particularly required, and the particle size of the emulsion droplets can be within the range.
According to the invention, glutaraldehyde, formaldehyde, melamine, urea and water are mixed for a second time to carry out polycondensation reaction, so as to obtain the melamine modified urea-formaldehyde resin prepolymer. In the present invention, the formaldehyde is preferably provided in the form of an aqueous formaldehyde solution; in the present invention, the mass concentration of the formalin is preferably 35 to 39%, and more preferably 37%. In the invention, the mass ratio of the glutaraldehyde to the formaldehyde is preferably 1: 1-3, and more preferably 1: 1.8-2.5; the mass ratio of the melamine to the urea is preferably 0.05-0.15: 1, and more preferably 0.08-0.12: 1. In the invention, the ratio of the total mass of glutaraldehyde and formaldehyde to the total mass of melamine and urea is preferably 2-4: 1, and more preferably 2.5-3: 1. The second mixing is not particularly limited as long as the second mixing can be uniformly mixed. In the present invention, it is preferable to further include, before the polycondensation reaction: and adjusting the pH value of the second mixed product to 7.5-8.5, and preferably 8. In the present invention, the pH adjusting agent for adjusting pH preferably includes triethanolamine or sodium hydroxide, more preferably triethanolamine. The invention has no special requirement on the dosage of the pH value regulator, as long as the pH value can be regulated to the required pH value. In the present invention, the polycondensation reaction is preferably accompanied by stirring, and the rotation speed of the stirring is preferably 200 to 400r/min, more preferably 260 to 320 r/min. In the invention, the temperature of the polycondensation reaction is preferably 60-90 ℃, and more preferably 70-80 ℃. In the present invention, the time of the polycondensation reaction is not particularly limited as long as the reaction system is formed into a colorless transparent solution.
After the capsule core material emulsion and the melamine modified urea-formaldehyde resin prepolymer are obtained, the melamine modified urea-formaldehyde resin prepolymer, the nano zinc oxide and the capsule core material emulsion are mixed for the third time, and the capsule wall crosslinking reaction is carried out, so that the energy storage and temperature regulation microcapsule is obtained. In the present invention, the third mixing preferably includes the steps of:
dispersing nano zinc oxide in the melamine modified urea-formaldehyde resin prepolymer to obtain a capsule wall material dispersion liquid;
mixing the capsule wall material dispersion liquid and the capsule core material emulsion.
The invention disperses nanometer zinc oxide in melamine modified urea-formaldehyde resin prepolymer to obtain capsule wall material dispersion. In the invention, the mass ratio of the nano zinc oxide to the total mass of the melamine and the urea is preferably 0.1-0.3: 1, and more preferably 0.16-0.25: 1. In the invention, the temperature of the dispersion is preferably 40-50 ℃, and more preferably 43-47 ℃. The dispersion method of the present invention is not particularly limited as long as the dispersion can be uniformly dispersed. The nano zinc oxide in the capsule wall material dispersion liquid of the invention endows the energy-storing and temperature-adjusting lyocell fiber with good antibacterial performance.
After the capsule core material emulsion and the capsule wall material dispersion are obtained, the capsule wall material dispersion and the capsule core material emulsion are mixed. In the invention, the mass ratio of the capsule core material to the melamine modified urea-formaldehyde resin prepolymer is preferably 1-2: 1, and more preferably 1.2-1.6: 1. In the invention, the mixing temperature is preferably 40-50 ℃, and more preferably 42-48 ℃. In the invention, the mixing is preferably carried out under the condition of stirring, and the rotating speed of the stirring is preferably 1800-2300 r/min, and more preferably 1980-2150 r/min. The stirring time is not particularly limited, and the stirring time is not particularly limited as long as the stirring time can be uniformly mixed.
In the invention, the temperature of the capsule wall crosslinking reaction is preferably 65-75 ℃, and more preferably 68-72 ℃; the time is preferably 150 to 240min, and more preferably 180 to 200 min.
According to the invention, the system after the capsule wall crosslinking reaction is preferably heated and evaporated to remove part of water, so that the mass percentage of the energy storage and temperature regulation microcapsules in the energy storage and temperature regulation microcapsule dispersion liquid is preferably 35-45%, and more preferably 38-42%. The heating evaporation is not specially limited, as long as the mass percentage of the energy storage temperature regulation microcapsule can be reached.
In the present invention, the capsule wall preferably further comprises, after the capsule wall crosslinking reaction: and carrying out solid-liquid separation on the system after the cross-linking reaction of the capsule wall to obtain the energy-storage temperature-regulating microcapsule. The solid-liquid separation is not particularly limited in the present invention as long as the solid-liquid separation can be achieved.
The invention preferably also comprises the following components before mixing the energy-storage temperature-regulating microcapsule, the cellulose pulp and the N-methylmorpholine-N-oxide aqueous solution: the cellulose pulp is activated. In the invention, the average polymerization degree of the cellulose pulp is preferably 600-800, and more preferably 680-750; the mass percentage content of alpha cellulose in the cellulose pulp is preferably 92-99%, and more preferably 96-98%. In the invention, the mass percentage content of the alpha cellulose in the spinning solution is preferably 10-20%, and more preferably 12-16%. In the invention, the activation is preferably cellulase activation, and the pH value of the activation is preferably 4-6, and more preferably 5-5.5; the temperature is preferably 40-55 ℃, and more preferably 45-50 ℃; the time is preferably 30 to 60min, and more preferably 40 to 50 min. In the invention, the mass ratio of the cellulase to the dry weight of the cellulose pulp is preferably 500-6000 g:1000kg, more preferably 2000-4000 g:1000 kg. In the present invention, it is preferable that the activation further comprises: and adjusting the pH value of the activated product to 10-12, and then squeezing. The pH regulator for regulating the pH value is not particularly limited, so long as the required pH value can be achieved. In the invention, the water content of the cellulose pulp after pressing is preferably 30-60%, and more preferably 40-50%.
In the present invention, the mass concentration of the aqueous solution of N-methylmorpholine-N-oxide is preferably 80 to 87%, more preferably 82 to 85%. In the invention, the mass ratio of the energy-storage temperature-regulating microcapsule to the cellulose pulp is preferably 18-50: 100, and more preferably 28-38: 100.
In order to simplify the operation, the invention preferably directly mixes the dispersion of the energy-storage and temperature-regulation microcapsule obtained after the capsule wall crosslinking reaction with the cellulose pulp and the N-methylmorpholine-N-oxide aqueous solution. In the invention, the mass concentration of the dispersion liquid of the energy-storage temperature-regulating microcapsule is preferably 35-45%, and more preferably 38-42%.
In the present invention, the post-treatment preferably includes heating, vacuuming, dehydrating, dissolving, homogenizing, deaerating and filtering, which are sequentially performed. The heating, vacuumizing, dehydrating, dissolving, homogenizing, defoaming and filtering are not particularly limited, and the conventional method in the field can be adopted.
After the spinning solution is obtained, the spinning solution is spun and then subjected to microwave treatment to obtain the energy-storage temperature-regulating lyocell fiber. In the invention, the spinning speed is preferably 35-45 m/min, and more preferably 40-42 m/min; the concentration of the coagulation bath for spinning is preferably 10-20%, and more preferably 13-18%; the temperature of the coagulating bath is preferably 15-25 ℃, and more preferably 18-22 ℃.
In the present invention, it is preferable that the microwave treatment further comprises: and (4) washing, bleaching and oiling the spinning product in sequence. In the invention, the water for washing is preferably deionized water, and the temperature of the water for washing is preferably 20-25 ℃, and more preferably 38-40 ℃.
In the invention, the bleaching is preferably aqueous solution bleaching of hydrogen peroxide, and the concentration of the aqueous solution of the hydrogen peroxide is preferably 1.0-2.0 g/L, more preferably 1.5-1.8 g/L; the pH value of the aqueous solution of the hydrogen peroxide is preferably 8.5-10, and more preferably 9-9.5; the temperature is preferably 30 to 45 ℃, and more preferably 36 to 41 ℃.
In the invention, the temperature of the oil bath for oiling is preferably 50-80 ℃, and more preferably 65-72 ℃; the pH value is preferably 6.0 to 9.0, more preferably 7.0 to 8.0. The oiling oil is not particularly limited, and the oil which is conventional in the field can be adopted. In the invention, the concentration of the oil in the oil bath is preferably 2.5-6.0 g/L, and more preferably 3.5-5.0 g/L.
In the invention, the microwave frequency of the microwave treatment is preferably 1560-1800 MHz, more preferably 1650-1720 MHz; the time of the microwave treatment is preferably 20-36 min, and more preferably 26-33 min.
In the microwave treatment, hydroxymethyl in the capsule wall of the energy-storing and temperature-regulating microcapsule and hydroxyl in cellulose are subjected to condensation polymerization to generate methylene bonds; meanwhile, hydrogen bonds are formed between unreacted hydroxymethyl and amino in the capsule wall and hydroxyl in the cellulose, so that the stability of the energy storage and temperature regulation microcapsule in the energy storage and temperature regulation lyocell fiber is improved.
In the present invention, the microwave treatment also serves to dry the cellulose fibers, and the moisture content of the cellulose fibers subjected to the microwave treatment is preferably 8.5 to 11.6%, and more preferably 9.7 to 10.2%.
The energy-storing and temperature-adjusting lyocell fiber provided by the invention can be applied to clothes or bedding.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
The embodiment of the invention has no limitation on the grade of the dosage of each raw material, and the raw materials can be prepared by adopting any weight grade as long as the raw materials are mixed according to a specific ratio.
Example 1
Melting paraffin at 40 ℃, and mixing with nano zinc oxide with the particle size of 50nm at the rotating speed of 600r/min to obtain a capsule core material; the mass ratio of the paraffin to the nano zinc oxide is 0.2: 10;
dispersing sodium styrene maleic anhydride in distilled water to obtain an emulsion dispersion liquid;
mixing the capsule core material and the emulsion dispersion liquid at the temperature of 40 ℃ and the rotating speed of 1800r/min to obtain capsule core material emulsion liquid; the capsule core material emulsion comprises 30 mass percent of capsule core material, 2.5 mass percent of sodium styrene maleic anhydride and 0.892 mu m of particle size D90;
mixing glutaraldehyde, 37% formaldehyde aqueous solution by mass concentration, melamine and urea, then adjusting the pH value of the mixture to 7.5 by using triethanolamine, and carrying out polycondensation reaction at the temperature of 60 ℃ and the rotating speed of 400r/min until a colorless transparent solution is formed, thereby obtaining a melamine modified urea-formaldehyde resin prepolymer solution; the mass ratio of the glutaraldehyde to the formaldehyde in the aqueous solution of formaldehyde is 1:1, the mass ratio of the melamine to the urea is 0.05:1, and the total mass ratio of the glutaraldehyde to the formaldehyde in the aqueous solution of formaldehyde to the melamine to the urea is 4: 1;
dispersing nano zinc oxide with the particle size of 50nm in melamine modified urea resin prepolymer solution at the temperature of 40 ℃ to obtain capsule wall material dispersion liquid; the total mass ratio of the nano zinc oxide to the melamine to the urea is 0.1: 1;
mixing the capsule core material emulsion and the capsule wall material dispersion at 40 ℃ and 1800r/min, and performing capsule wall crosslinking reaction at 65 ℃ for 240min to obtain an energy storage temperature regulation microcapsule dispersion; wherein the mass ratio of the obtained capsule core material to the melamine modified urea-formaldehyde resin prepolymer is 1: 1; heating and evaporating to obtain an energy storage and temperature regulation microcapsule dispersion liquid with the mass concentration of 35%;
performing cellulase activation on cellulose pulp with the average polymerization degree of 600 and the content of 92 percent by mass of alpha cellulose at the pH value of 4 and the temperature of 40 ℃ for 60min, wherein the mass ratio of the cellulase to the dry weight of the cellulose pulp is 500g:1000 kg; adjusting the pH value to 10 after activation, and squeezing to obtain cellulose pulp with the water content of 30 wt%;
mixing the energy-storage and temperature-adjustment microcapsule dispersion liquid, the squeezed cellulose pulp and an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 80%, and then sequentially heating, vacuumizing, dehydrating, dissolving, homogenizing, defoaming and filtering to obtain a spinning stock solution; wherein the mass ratio of the energy storage and temperature adjustment microcapsules to the cellulose pulp is 18:100, and the mass percentage content of alpha cellulose in the spinning solution is 10%;
spinning the spinning stock solution, and then sequentially washing (deionized water, 20 ℃), bleaching (hydrogen peroxide aqueous solution with the concentration of 1.0g/L, pH value of 8.5, temperature of 45 ℃) and oiling (oil bath concentration of 2.5g/L, temperature of 50 ℃, pH value of 6.0), and then carrying out microwave treatment for 36min at 1560MHz to obtain the energy-storage temperature-adjusting lyocell fiber with the water content of 8.5% and the specification of 2.22dtex 38 mm; wherein the spinning speed is 35m/min, the concentration of the coagulation bath for spinning is 10 percent, and the temperature of the coagulation bath is 15 ℃.
Example 2
Melting octadecane at 42 ℃, and mixing with nano zinc oxide with the particle size of 38nm at the rotating speed of 680r/min to obtain a capsule core material; the mass ratio of the paraffin to the nano zinc oxide is 0.25: 1;
dispersing span-80 in distilled water to obtain an emulsion dispersion liquid;
mixing the capsule core material and the emulsion dispersion liquid at 42 ℃ and the rotation speed of 1980r/min to obtain capsule core material emulsion liquid; the capsule core material emulsion comprises 32.5% of capsule core material by mass, 3.2% of span-80 by mass and 0.952 μm of particle size D90;
mixing glutaraldehyde, 37% formaldehyde aqueous solution by mass concentration, melamine and urea, then adjusting the pH value of the mixture to 8.0 by using triethanolamine, and carrying out polycondensation reaction at the temperature of 70 ℃ and the rotating speed of 320r/min until a colorless transparent solution is formed, thereby obtaining a melamine modified urea-formaldehyde resin prepolymer solution; the mass ratio of the glutaraldehyde to the formaldehyde in the aqueous solution of formaldehyde is 1:1.8, the mass ratio of the melamine to the urea is 0.08:1, and the total mass ratio of the glutaraldehyde to the formaldehyde in the aqueous solution of formaldehyde to the melamine to the urea is 3: 1;
dispersing nano zinc oxide with the particle size of 35nm in melamine modified urea-formaldehyde resin prepolymer solution at the temperature of 43 ℃ to obtain capsule wall material dispersion liquid; the total mass ratio of the nano zinc oxide to the melamine to the urea is 0.16: 1;
mixing the capsule core material emulsion and the capsule wall material dispersion at 42 ℃ and the rotation speed of 1980r/min, and performing capsule wall crosslinking reaction at 68 ℃ for 200min to obtain an energy storage temperature regulation microcapsule dispersion; wherein the mass ratio of the obtained capsule core material to the melamine modified urea-formaldehyde resin prepolymer is 1.2: 1; heating and evaporating to obtain an energy storage and temperature regulation microcapsule dispersion liquid with the mass concentration of 38%;
cellulose pulp with average polymerization degree of 680 and mass percent of alpha cellulose of 96 percent is subjected to cellulase activation for 50min at the temperature of 45 ℃ and the pH value of 5, and the mass ratio of the cellulase to the dry weight of the cellulose pulp is 2000 g:1000 kg; adjusting the pH value to 10.5 after activation, and squeezing to obtain cellulose pulp with the water content of 40 wt%;
mixing the energy-storage and temperature-adjustment microcapsule dispersion liquid, the squeezed cellulose pulp and an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 82%, and then sequentially heating, vacuumizing, dehydrating, dissolving, homogenizing, defoaming and filtering to obtain a spinning stock solution; wherein the mass ratio of the energy storage and temperature adjustment microcapsules to the cellulose pulp is 28:100, and the mass percentage content of alpha cellulose in the spinning stock solution is 12%;
spinning the spinning stock solution, and then sequentially washing with water (deionized water, 30 ℃), bleaching (hydrogen peroxide aqueous solution with the concentration of 1.5g/L, pH value of 9.0, temperature of 41 ℃) and oiling (oil bath concentration of 3.5g/L, temperature of 70 ℃, pH value of 7.0), and then carrying out microwave treatment for 33min at 1650MHz to obtain the energy-storage temperature-regulating lyocell fiber with the water content of 9.7% and the specification of 3.33dtex 42 mm; wherein the spinning speed is 40m/min, the concentration of the coagulation bath for spinning is 13%, and the temperature of the coagulation bath is 18 ℃.
Example 3
Melting n-nonadecane at 48 ℃, and mixing with nano zinc oxide with the particle size of 25nm at the rotating speed of 800r/min to obtain a capsule core material; the mass ratio of the paraffin to the nano zinc oxide is 0.28: 1;
dispersing sodium dodecyl sulfate in distilled water to obtain an emulsion dispersion liquid;
mixing the capsule core material and the emulsion dispersion liquid at the temperature of 46 ℃ and the rotating speed of 21150r/min to obtain capsule core material emulsion liquid; the capsule core material emulsion comprises 36.8% of capsule core material by mass, 3.75% of sodium dodecyl sulfate by mass and 0.998 μm of particle size D90;
mixing glutaraldehyde, 37% formaldehyde aqueous solution by mass concentration, melamine and urea, adjusting the pH value of the mixture to 8.0 by using sodium hydroxide, and carrying out polycondensation reaction at the temperature of 80 ℃ and the rotating speed of 260r/min until a colorless transparent solution is formed to obtain a melamine modified urea-formaldehyde resin prepolymer solution; the mass ratio of the glutaraldehyde to the formaldehyde in the aqueous solution of formaldehyde is 1:2.5, the mass ratio of the melamine to the urea is 0.12:1, and the total mass ratio of the glutaraldehyde to the formaldehyde in the aqueous solution of formaldehyde to the melamine to the urea is 2.5: 1;
dispersing nano zinc oxide with the particle size of 20nm in a melamine modified urea-formaldehyde resin prepolymer solution at the temperature of 47 ℃ to obtain a capsule wall material dispersion liquid; the total mass ratio of the nano zinc oxide to the melamine to the urea is 0.25: 1;
mixing the capsule core material emulsion and the capsule wall material dispersion at the temperature of 48 ℃ and the rotating speed of 2150r/min, and then carrying out capsule wall crosslinking reaction at 72 ℃ for 180min to obtain an energy-storing and temperature-adjusting microcapsule dispersion; wherein the mass ratio of the obtained capsule core material to the melamine modified urea-formaldehyde resin prepolymer is 1.6: 1; heating and evaporating to obtain an energy storage and temperature regulation microcapsule dispersion liquid with the mass concentration of 42%;
cellulose pulp with the average polymerization degree of 750 and the mass percentage content of alpha cellulose of 98 percent is subjected to cellulose activation for 40min at the temperature of 50 ℃ and the pH value of 5.5, and the mass ratio of the cellulose to the dry weight of the cellulose pulp is 4000 g:1000 kg; adjusting the pH value to 11.5 after activation, and squeezing to obtain cellulose pulp with the water content of 50 wt%;
mixing the energy-storage and temperature-adjustment microcapsule dispersion liquid, the squeezed cellulose pulp and an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 85%, and then sequentially heating, vacuumizing, dehydrating, dissolving, homogenizing, defoaming and filtering to obtain a spinning stock solution; wherein the mass ratio of the energy storage and temperature adjustment microcapsules to the cellulose pulp is 38:100, and the mass percentage content of alpha cellulose in the spinning stock solution is 16%;
spinning the spinning stock solution, and then sequentially performing water washing (deionized water, 40 ℃), bleaching (hydrogen peroxide aqueous solution with the concentration of 1.8g/L, pH value of 9.5, temperature of 36 ℃) and oiling (oil bath concentration of 5.0g/L, temperature of 65 ℃, pH value of 8.0), and performing microwave treatment for 26min at 1720MHz to obtain the energy storage temperature-adjusting lyocell fiber with the water content of 10.2% and 5.56dtex 60 mm; wherein the spinning speed is 42m/min, the concentration of the coagulation bath for spinning is 18 percent, and the temperature of the coagulation bath is 22 ℃.
Example 4
Melting n-eicosane at 50 ℃, and mixing the melted n-eicosane with nano zinc oxide with the particle size of 15nm at the rotating speed of 850r/min to obtain a capsule core material; the mass ratio of the paraffin to the nano zinc oxide is 0.3: 1;
dispersing tween-80 in distilled water to obtain emulsion dispersion;
mixing the capsule core material and the emulsion dispersion liquid at the temperature of 50 ℃ and the rotating speed of 2300r/min to obtain capsule core material emulsion liquid; the capsule core material emulsion comprises 40% of capsule core material by mass, 4% of tween-80 by mass and 1.055 mu m of particle size D90;
mixing glutaraldehyde, 37 mass percent aqueous formaldehyde solution, melamine and urea, adjusting the pH value of the mixture to 8.5 by using sodium hydroxide, and carrying out polycondensation reaction at the temperature of 90 ℃ and the rotating speed of 200r/min until colorless transparent solution is formed to obtain melamine modified urea-formaldehyde resin prepolymer solution; the mass ratio of the glutaraldehyde to the formaldehyde in the aqueous solution of formaldehyde is 1:3, the mass ratio of the melamine to the urea is 0.15:1, and the total mass ratio of the glutaraldehyde to the formaldehyde in the aqueous solution of formaldehyde to the melamine to the urea is 2: 1;
dispersing nano zinc oxide with the particle size of 15nm in a melamine modified urea-formaldehyde resin prepolymer solution at the temperature of 50 ℃ to obtain a capsule wall material dispersion liquid; the total mass ratio of the nano zinc oxide to the melamine to the urea is 0.3: 1;
mixing the capsule core material emulsion and the capsule wall material dispersion at the temperature of 50 ℃ and the rotation speed of 2300r/min, and then carrying out capsule wall crosslinking reaction at the temperature of 75 ℃ for 150min to obtain an energy storage temperature regulation microcapsule dispersion; wherein the mass ratio of the obtained capsule core material to the melamine modified urea-formaldehyde resin prepolymer is 2: 1; heating and evaporating to obtain an energy storage and temperature regulation microcapsule dispersion liquid with the mass concentration of 45%;
cellulose pulp with the average polymerization degree of 800 and the content of 99 percent of alpha cellulose by weight is subjected to cellulase activation for 30min at the temperature of 55 ℃ and the pH value of 6, and the mass ratio of the cellulase to the dry weight of the cellulose pulp is 6000 g:1000 kg; adjusting the pH value to 12 after activation, and squeezing to obtain cellulose pulp with the water content of 60 wt%;
mixing the energy-storage and temperature-adjustment microcapsule dispersion liquid, the squeezed cellulose pulp and an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 87%, and then sequentially heating, vacuumizing, dehydrating, dissolving, homogenizing, defoaming and filtering to obtain a spinning stock solution; wherein the mass ratio of the energy storage and temperature adjustment microcapsules to the cellulose pulp is 50:100, and the mass percentage content of alpha cellulose in the spinning solution is 20%;
spinning the spinning stock solution, and then sequentially washing with water (deionized water, 50 ℃), bleaching (a hydrogen peroxide aqueous solution with the concentration of 2.0g/L, the pH value of 10.0 and the temperature of 30 ℃) and oiling (an oil bath with the concentration of 6.0g/L, the temperature of 65 ℃ and the pH value of 9.0), and then carrying out microwave treatment for 20min at 1800MHz to obtain the energy-storage temperature-regulating lyocell fiber with the water content of 11.6% and the specification of 6.67dtex 60 mm; wherein the spinning speed is 45m/min, the concentration of the coagulation bath for spinning is 20%, and the temperature of the coagulation bath is 25 ℃.
The dry breaking strength, the wet breaking strength and the transverse swelling rate of the energy storage temperature-regulating lyocell fibers prepared in examples 1 to 4 were measured according to GB/T14337-2008 "test method for tensile properties of chemical fiber staple fibers", and the results are shown in Table 1.
According to part 3 of GBT 20944.3-2008 evaluation of antibacterial performance of textiles: the oscillation method detects the inhibition rate of the energy-storage and temperature-adjustment lyocell fibers prepared in examples 1 to 4 on staphylococcus aureus, escherichia coli and candida albicans, and the results are shown in table 1.
According to GB/T19466.3-2004, Differential Scanning Calorimetry (DSC) of plastics, part 3: the measurement of melting and crystallization temperatures and enthalpies "examined the phase transition melting temperature, melting phase transition enthalpy, phase transition crystallization temperature, and crystallization phase transition enthalpy of the energy storage temperature-controlled lyocell fibers prepared in examples 1 to 4, and the results are shown in table 1.
Table 1 performance parameters of the energy storage and temperature regulation lyocell fibers prepared in examples 1 to 4
As can be seen from Table 1, the energy-storing and temperature-adjusting lyocell fiber provided by the invention has excellent tensile property and antibacterial property; meanwhile, the energy storage and temperature regulation lyocell fiber provided by the invention has high-efficiency energy storage and temperature regulation performance.
According to the standard FZ/T73023-2006 appendix C4. simplified washing conditions and washing methods in the procedure, the energy storage temperature-adjusting lyocell fibers prepared in examples 1-4 were washed 50 times and then subjected to performance testing, and the results are listed in Table 2.
Table 2 performance parameters of the energy storage and temperature adjustment lyocell fibers prepared in examples 1 to 4 after being washed 50 times
As can be seen from Table 2, the energy storage and temperature regulation lyocell fiber provided by the invention still has excellent tensile property and antibacterial property and high-efficiency energy storage and temperature regulation performance after being washed for multiple times.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (10)
1. The energy-storage and temperature-regulation lyocell fiber comprises lyocell fibers and energy-storage and temperature-regulation microcapsules crosslinked with the lyocell fibers, wherein the energy-storage and temperature-regulation microcapsules comprise a capsule wall and a capsule core, the capsule core comprises a phase change material and a nano nucleating agent, and the capsule wall comprises melamine modified urea-formaldehyde resin prepolymer.
2. The energy storage and temperature regulation lyocell fiber according to claim 1, wherein the mass ratio of the lyocell fiber to the energy storage and temperature regulation microcapsule is 100: 17.5 to 49.0.
3. The energy-storing and temperature-regulating lyocell fiber according to claim 1, wherein the capsule wall further comprises nano zinc oxide.
4. The energy storing and temperature regulating lyocell fiber of claim 1, wherein said phase change material comprises paraffin, n-octadecane, n-nonadecane, or n-eicosane;
the nano nucleating agent comprises nano zinc oxide, nano titanium dioxide, nano calcium carbonate or nano silicon dioxide; the grain size of the nano nucleating agent is 15-50 nm;
the mass ratio of the nano nucleating agent to the phase-change material is 0.2-0.3: 10.
5. The energy-storing and temperature-adjusting lyocell fiber as claimed in claim 3, wherein the mass ratio of the nano zinc oxide to the melamine modified urea-formaldehyde resin prepolymer is 0.1-0.3: 1.
6. A method for preparing the energy-storing and temperature-adjusting lyocell fiber according to any one of claims 1 to 5, comprising the steps of:
mixing the energy-storage temperature-regulating microcapsule, the cellulose pulp and the N-methylmorpholine-N-oxide aqueous solution, and then carrying out post-treatment to obtain a spinning stock solution;
and carrying out microwave treatment on the spinning stock solution after spinning to obtain the energy-storage temperature-regulating lyocell fiber.
7. The preparation method according to claim 6, wherein the microwave treatment is carried out at a microwave frequency of 1560-1800 MHz for a period of 20-36 min.
8. The preparation method according to claim 6, wherein the mass percentage of the alpha cellulose in the cellulose pulp is 92-99%, and the mass ratio of the energy storage and temperature regulation microcapsule to the cellulose pulp is 18-50: 100.
9. The preparation method according to claim 6 or 8, wherein the preparation method of the energy storage and temperature regulation microcapsule comprises the following steps:
firstly mixing the phase change material, the nano nucleating agent, the emulsifier and water to obtain capsule core material emulsion;
mixing glutaraldehyde, formaldehyde, melamine, urea and water for a second time, and carrying out polycondensation reaction to obtain a melamine modified urea-formaldehyde resin prepolymer;
and thirdly, mixing the melamine modified urea-formaldehyde resin prepolymer, the nano zinc oxide and the capsule core material emulsion for carrying out capsule wall crosslinking reaction to obtain the energy-storage temperature-regulating microcapsule.
10. The method according to claim 9, wherein the temperature of the polycondensation reaction is 40 to 50 ℃;
the temperature of the capsule wall crosslinking reaction is 65-75 ℃; the time is 150-240 min.
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