CN111485428B - Heat-accumulating temperature-regulating textile and preparation method thereof - Google Patents
Heat-accumulating temperature-regulating textile and preparation method thereof Download PDFInfo
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- CN111485428B CN111485428B CN201910072864.7A CN201910072864A CN111485428B CN 111485428 B CN111485428 B CN 111485428B CN 201910072864 A CN201910072864 A CN 201910072864A CN 111485428 B CN111485428 B CN 111485428B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D—TEXTILES; PAPER
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
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- D—TEXTILES; PAPER
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
- D06M13/5135—Unsaturated compounds containing silicon atoms
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/20—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin
- D06M14/22—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
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- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/20—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin
- D06M14/24—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of natural origin of animal origin, e.g. wool or silk
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/32—Polyesters
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- D—TEXTILES; PAPER
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- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/34—Polyamides
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- D—TEXTILES; PAPER
- 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
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- 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
- D06M2101/10—Animal fibres
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- 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
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/14—Thermal energy storage
Abstract
The invention discloses a heat-accumulating temperature-regulating textile and a preparation method thereof, wherein the heat-accumulating temperature-regulating textile is prepared by coating a mixture consisting of modified phase-change microcapsules, organic monomer dispersion medium and initiator on the surface of a textile substrate to form a coating, wherein the modified phase-change microcapsules are prepared by modifying phase-change microcapsules taking silicon dioxide as a shell layer and phase-change materials as core materials by a silane coupling agent. The heat-accumulating temperature-regulating textile overcomes the problem of poor firmness between the phase-change microcapsules and the textile base material, and the prepared heat-accumulating temperature-regulating textile has the advantages of good washing fastness, high latent heat, uniform temperature regulation and the like, and meanwhile, the preparation method has the characteristics of low equipment requirement, easy control of reaction process, simple operation, rapid molding and the like.
Description
Technical Field
The invention belongs to the technical field of functional textile preparation, in particular to an intelligent textile, and more particularly relates to a heat-accumulating temperature-regulating textile and a preparation method thereof.
Background
With the progress of human society and the increasing level of living, people are favored for intelligent textiles with some special functions. The heat-accumulating temperature-regulating textile is a novel intelligent textile capable of releasing energy when the ambient temperature is low and absorbing heat after the ambient temperature is high, has the function of bidirectional temperature regulation, can automatically absorb, store, distribute and release energy, and brings close attention to textile dyeing and finishing workers. At present, the heat-accumulating temperature-regulating textile has great application prospect in the fields of military, clothing, bedding, medical supplies and the like.
The heat accumulating and temperature regulating textile can be prepared by applying microencapsulated phase change materials on textile substrates, and has been widely reported in recent years, such as a heat accumulating and temperature regulating textile disclosed in Chinese patent No. 201611109749.5, no. CN200710057493.2 and No. CN201410407505. X. Generally, the phase-change microcapsules are mainly applied to textiles in a spinning method and a finishing method. The spinning method is to spin the phase-change microcapsule as the component of the spinning solution, which has strict requirements on the particle size, acid and alkali resistance and heat resistance of the phase-change microcapsule, and has a plurality of operation procedures and higher requirements on equipment; the after-finishing method is characterized in that the phase-change microcapsule is used as a finishing liquid component and is treated on the surface of the textile in a dipping, padding or coating mode, the operation is simple, the requirement on equipment is low, the method is a conventional method for preparing the phase-change microcapsule heat-accumulating temperature-regulating textile at present, and the prepared phase-change microcapsule material is mixed with an adhesive and then coated on the surface of the textile to prepare the intelligent temperature-regulating textile, for example, the phase-change microcapsule material is prepared in China patent No. 200710057493.2.
However, when the phase-change microcapsule is treated on the textile by adopting the after-treatment method, the combination fastness between the phase-change microcapsule and the textile substrate is weak, and the phase-change microcapsule is easy to fall off, so that the practical application of the phase-change microcapsule heat-storage temperature-adjustment textile is greatly limited. Therefore, it is urgent to obtain the heat-accumulating temperature-regulating textile with good combination fastness between the phase-change microcapsule and the substrate.
Disclosure of Invention
The group discovers that the phase-change microcapsule taking silicon dioxide as a shell layer and a phase-change material as a core material is modified to form the reactive modified phase-change microcapsule with double bonds on the surface, the obtained mixture of the modified phase-change microcapsule, an organic monomer dispersion medium and an initiator is coated on the surface of a textile substrate, and the heat-storage temperature-regulating textile with good bonding fastness and stability can be obtained after curing treatment, so that the aim of forming stable bonding between the phase-change microcapsule and the textile substrate is fulfilled.
The first object of the invention is to provide a heat accumulating and temperature regulating textile.
Preferably, the heat-accumulating temperature-regulating textile is prepared by coating a mixture consisting of modified phase-change microcapsules, an organic monomer dispersion medium and an initiator on the surface of a textile substrate to form a coating, wherein the modified phase-change microcapsules are prepared by modifying phase-change microcapsules with silicon dioxide serving as a shell layer and a phase-change material serving as a core material by a silane coupling agent.
The preparation method of the phase-change microcapsule taking silicon dioxide as a shell layer and phase-change material as a core material and the method for modifying the phase-change microcapsule by using the silane coupling agent are not particularly limited, and the preparation and modification of the phase-change microcapsule can be carried out by adopting a mode well known to a person skilled in the art.
The coating method and the equipment used for the coating are not particularly limited in the present invention, and the coating method and the coating equipment well known to those skilled in the art, such as a doctor blade coater, may be used for the coating.
Preferably, the composition of the mixed solution is 100 parts of organic monomer dispersion medium, 5-15 parts of modified phase-change microcapsule emulsion and 0.5-1 part of initiator.
Preferably, the phase change material is any one of paraffin, fatty acid and fatty alcohol or a mixture eutectic of any two or more of the paraffin, fatty acid and fatty alcohol, wherein the phase change temperature of the phase change material is 22-40 ℃.
Preferably, the organic monomer dispersion medium is any one of hydroxyethyl acrylate and hydroxypropyl acrylate.
Preferably, the silane coupling agent is any one of gamma- (methacryloxy) propyl trimethoxy silane, vinyl trimethoxy silane, triethoxy vinyl and vinyl tri (b-methoxyethoxy) silane.
The silane coupling agent has one end with reactive double bond and the other end with silica bond, and silanol formed by methoxy hydrolysis of the silane coupling agent can react with silicon hydroxyl of silicon dioxide to generate Si-O-Si bond, so that the silane coupling agent is connected to the surface of the silicon dioxide, and the phase-change microcapsule taking the silicon dioxide as a shell layer is modified into a reactive phase-change microcapsule. The active double bond at the other end of the reactive phase-change microcapsule is polymerized with an organic monomer under the catalysis of an initiator, so that the textile substrate is used as an in-situ point to be solidified into a film on the surface of the textile substrate.
Preferably, the initiator is a photoinitiator, including an ultraviolet initiator or a blue photoinitiator.
Preferably, the ultraviolet initiator is any one of 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-acetone and azodiisobutyronitrile.
Preferably, the blue photoinitiator is any one of 1-phenyl-1, 2-propanedione and 4- (dimethylamino) ethyl benzoate.
When the initiator is a photoinitiator, the light fixing technology is adopted to carry out curing and film forming, and the specific principle is that the photoinitiator absorbs ultraviolet light or visible light radiation energy to initiate the polymerization of monomers in the mixed solution and rapidly form a cured film layer.
It will be appreciated that the initiator according to the present invention may be a thermal initiator and that when the initiator is a thermal initiator, curing to a film is effected using a thermal curing technique, such as oven drying, which is common.
As a preferred mode, the invention adopts a photoinitiator and a photocuring mode, and the mixed solution coated on the surface of the textile substrate can be changed from a liquid state to a solid state in a few minutes by adopting the preferred mode, so that the defects of slow film formation and low efficiency in a heat fixing mode are effectively overcome.
Preferably, the textile substrate is any one of cotton, silk, terylene, polyester cotton, modal, tencel fabric, polypropylene non-woven fabric and polyester non-woven fabric.
The second aim of the invention is to provide a preparation method of the heat-accumulating temperature-regulating textile.
Preferably, the preparation method of the heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of modified phase-change microcapsules: ultrasonically dispersing phase-change microcapsule emulsion taking silicon dioxide as a shell layer and a phase-change material as a core material for 15min, adding a silane coupling agent which accounts for 10-15% of the mass of the phase-change microcapsule emulsion and is pre-hydrolyzed, placing the obtained mixed solution into a reaction kettle at 70-80 ℃, reacting for 3-6 h at a stirring speed of 200-300 r/min, discharging, and filtering to obtain the modified phase-change microcapsule;
(2) Preparing a heat-accumulating temperature-regulating textile: and (3) performing ultrasonic dispersion on a mixed solution consisting of an organic monomer dispersion medium, a modified phase-change microcapsule emulsion and an initiator for 15min, coating the mixed solution on the surface of a textile substrate, and performing curing treatment to obtain the heat-accumulating temperature-regulating textile.
Preferably, the composition of the mixed solution is 100 parts of organic monomer dispersion medium, 5-15 parts of modified phase-change microcapsule emulsion and 0.5-1 part of initiator.
Preferably, the initiator in the step (2) is a photoinitiator, and the curing treatment is a curing treatment under irradiation of a light source for 1 to 5 minutes.
Preferably, the light source is an ultraviolet high-pressure mercury lamp with the power of 250W and the central wavelength at 365nm or a blue LED lamp with the power of 200W and the central wavelength at 425 nm.
Preferably, the phase change material is any one of paraffin, fatty acid and fatty alcohol or a mixture eutectic of any two or more of the paraffin, fatty acid and fatty alcohol, wherein the phase change temperature of the phase change material is 22-40 ℃.
Preferably, the organic monomer dispersion medium is any one of hydroxyethyl acrylate and hydroxypropyl acrylate.
Preferably, the silane coupling agent is any one of gamma- (methacryloxy) propyl trimethoxy silane, vinyl trimethoxy silane, triethoxy vinyl and vinyl tri (b-methoxyethoxy) silane.
Preferably, the initiator is a photoinitiator, including an ultraviolet initiator or a blue photoinitiator.
Preferably, the ultraviolet initiator is any one of 2,4, 6-trimethyl benzoyl-diphenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-acetone and azo diisobutyronitrile.
Preferably, the blue photoinitiator is any one of 1-phenyl-1, 2-propanedione and 4- (dimethylamino) ethyl benzoate.
Preferably, the textile substrate is any one of cotton, silk, terylene, polyester cotton, modal, tencel fabric, polypropylene non-woven fabric and polyester non-woven fabric.
The beneficial results are as follows:
(1) The invention utilizes silane coupling agent to modify phase-change microcapsule taking silicon dioxide as shell layer to obtain modified phase-change microcapsule with active double bond on surface, the mixture composed of modified phase-change microcapsule, organic monomer dispersion medium and initiator is coated on the surface of textile base material, and the initiator is used for catalyzing and modifying phase-change microcapsule and organic monomer to make polymerization reaction so as to form phase-change microcapsule solidified film layer on the surface of textile base material and obtain the invented textile with heat-accumulating and temperature-regulating property.
(2) The phase-change microcapsule is solidified on the surface of the textile substrate to form a film by adopting the photoinitiator and the light fixing mode, and the phase-change microcapsule has the advantages of high film forming speed, low equipment requirement, easy control of the reaction process, simplicity in operation, environment friendliness, good universality and the like.
The raw materials for preparing the heat-accumulating temperature-regulating textile have the following functions:
1. phase-change microcapsule
The phase change microcapsule is a composite phase change material with a core-shell structure, which is formed by coating a layer of film with stable performance on the surface of phase change material particles by utilizing microcapsule technology, so that the environment where the phase change material forming the core material is positioned is more stable and is not influenced by external environmental factors. After the phase-change microcapsule is arranged on the textile substrate, the phase-change material serving as the core material is subjected to liquid-solid reversible change along with the change of the external environment temperature, namely, absorbs and stores heat when the environment temperature is increased, and is changed from solid to liquid; when the ambient temperature is reduced, the stored heat is released, and the textile changes from a liquid state to a solid state, so that the temperature self-adjustment of the textile is realized. The phase-change microcapsule taking silicon dioxide as a shell layer has wide application in the textile field, and the phase-change microcapsule has the advantages of good thermal conductivity and no oil immersion negative influence on the appearance of the fabric when heat absorption and melting occur, but has the defect of poor bonding fastness with the fabric.
In the invention, the inventor utilizes a silane coupling agent to modify phase-change microcapsules taking silicon dioxide as a shell layer, and the main principle is as follows: one end of the silane coupling agent is a reactive double bond, the other end is a silicon-oxygen bond, silanol formed by methoxy hydrolysis of the silane coupling agent can generate Si-O-Si bond with silicon hydroxyl of silicon dioxide through dehydration reaction, and the silanol is connected to the surface of the silicon dioxide, so that the phase-change microcapsule taking the silicon dioxide as a shell layer is modified into the reactive phase-change microcapsule with the active double bond. The active double bonds on the surface of the modified phase-change microcapsule can carry out polymerization reaction with an organic monomer, so that a stable film layer can be formed on the surface of a textile substrate, and the bonding fastness of the phase-change microcapsule and the textile substrate is enhanced.
2. Organic monomer dispersion medium
The organic monomer dispersion medium is a main substance in a polymerization system, and belongs to a reactant in the polymerization system together with the modified phase-change microcapsule, and can be polymerized in situ on a textile substrate to form a film with stronger adhesiveness. Hydroxyethyl acrylate and hydroxypropyl acrylate are two common organic monomers, the polymerization performance is good, and the obtained film is transparent and has better flexibility; in addition, hydroxyl groups which can form hydrogen bond function are also arranged in the molecular structures of the hydroxyethyl acrylate and the hydroxypropyl acrylate, so that the adhesion between the obtained film and the textile substrate is further enhanced.
3. Initiator(s)
The initiator plays a role in catalyzing polymerization reaction in a polymerization system, and common initiators are thermal initiators and photoinitiators. Wherein the thermal initiator initiates polymerization by generating free radicals by thermal cleavage, and widely used thermal initiators include peroxides and azo compounds; the photoinitiator is a photoinitiator which absorbs photon energy to generate free radicals to initiate polymerization after light irradiation, and widely used photoinitiators comprise ultraviolet light initiators and blue light initiators. In the invention, both the thermal initiator and the photoinitiator are suitable for preparing the heat accumulating and temperature regulating textile. In a preferred embodiment, the photoinitiator is used for catalyzing the polymerization of the phase-change microcapsule and the organic monomer, and the phase-change microcapsule film layer is rapidly formed on the textile substrate in a photo-curing mode, so that the defects of low film forming efficiency, difficult control of the film forming process and the like in a thermal curing mode are overcome.
Drawings
Fig. 1 is a scanning electron microscope (FESEM) image of the phase-change microcapsule prepared in example 1 of the present invention.
Fig. 2 is a scanning electron microscope (FESEM) image at 1000 x magnification of the heat accumulating temperature regulating cotton fabric of example 1 of the present invention.
FIG. 3 is a Differential Scanning Calorimeter (DSC) curve of the phase-change microcapsule heat-storage temperature-adjustment cotton fabric prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in more detail with reference to examples. It should be understood that the practice of the invention is not limited to the following examples, but is intended to be within the scope of the invention in any form and/or modification thereof.
In the present invention, unless otherwise specified, all parts and percentages are by weight, all equipment, materials, etc. are commercially available or are commonly used in the industry. The methods employed in the examples are those generally known in the art, unless otherwise indicated.
In the invention, the following equipment is used for testing the surface morphology and heat storage performance of the phase-change microcapsule and the heat storage temperature-regulating textile: the surface morphology of the dried and metal-sprayed phase-change microcapsules and the heat-accumulating temperature-regulating textile are observed by using an ULTRA55 scanning electron microscope of the German zeiss company. And (3) under the protection of nitrogen, a Differential Scanning Calorimeter (DSC) of Q2000 of TA company in the United states is adopted, the temperature is increased from-10 ℃ to 50 ℃ at the speed of 10 ℃/min, the temperature is kept for 1 minute and then is reduced to-10 ℃, the DSC curve of the test process is recorded, and the phase transition temperature and the latent heat value of the phase transition microcapsule and the heat-storage temperature-regulating textile are calculated and obtained.
Example 1
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: taking paraffin as a phase-change core material, SDS as an emulsifying agent, taking water as a dispersion medium, starting high-speed emulsification for 30min, taking out, pouring into a 500ml three-neck flask, adding ammonia water, setting a constant-temperature reaction condition at 40 ℃, adding tetraethoxysilane and ethanol into the reaction flask, setting a stirring rate of 260r/min, taking out from the flask after stirring for 24h, and obtaining the phase-change microcapsule taking silicon dioxide as a shell layer.
(2) Modification of phase-change microcapsules: taking 100g of phase-change microcapsule emulsion taking silicon dioxide as a shell layer and paraffin as a core material, performing ultrasonic dispersion for 15min, then adding 10g of gamma- (methacryloyloxy) propyl trimethoxysilane which is subjected to ultrasonic prehydrolysis for 15min in 40 parts of water, placing the mixed solution in a reaction kettle at 70 ℃, setting the stirring speed of 200r/min, discharging after reacting for 3h, and filtering to obtain the modified phase-change microcapsule emulsion for later use.
(3) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm x 10cm (length x width), 100g of hydroxyethyl acrylate dispersion medium, 5g of modified phase-change microcapsule emulsion and 0.5g of ultraviolet light initiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide.
(4) Preparing a heat-accumulating temperature-regulating textile: and ultrasonically dispersing the mixed solution consisting of the hydroxyethyl acrylate dispersion medium, the modified phase-change microcapsule emulsion and the ultraviolet initiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide for 15min, then applying the mixed solution to the surface of pure cotton fabric, vertically clamping the cotton fabric with the reaction solution applied by two transparent glass plates, irradiating for 1min under a 250W ultraviolet high-pressure mercury lamp, and taking out the treated cotton fabric to obtain the phase-change microcapsule heat-storage temperature-regulating textile.
And (3) carrying out water washing test on the obtained phase-change microcapsule heat-storage temperature-regulating textile, and representing the adhesiveness of the phase-change microcapsule on the textile by testing the weight and latent heat value change condition of the heat-storage temperature-regulating textile before and after water washing. Soaking and washing the phase-change microcapsule heat-accumulating temperature-regulating textile in warm water at 45 ℃ for 2min, taking out and wringing out the textile to be washed for 1 time, and then analogically, washing for 10 times and 20 times, and then respectively carrying out weighing and differential scanning calorimeter testing.
FIG. 1 is a scanning electron microscope (FESEM) image of the prepared phase-change microcapsules, which were found to have smooth surfaces; FIG. 2 is a scanning electron microscope (FESEM) image of a heat accumulating temperature regulating cotton fabric, showing that the microcapsules have significantly adhered to the cotton fabric; FIG. 3 is a Differential Scanning Calorimeter (DSC) curve of the phase-change microcapsule heat-storage temperature-adjustment cotton fabric prepared in example 1 of the present invention. Through detection, the phase-change latent heat value is 110J/g, the weight gain of the heat-storage temperature-regulating cotton fabric is 28.5%, the melting phase-change temperature is 27.8 ℃, the phase-change latent heat is 30.4J/g, and after ultraviolet light curing, the reactive phase-change microcapsule is obviously attached to the cotton fabric. After washing for 10 times, the weight gain of the heat accumulating and temperature regulating cotton fabric is 28.1 percent, and the phase change latent heat is 30.1J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are not changed greatly after the textile is subjected to comparative washing for 10 times, which indicates that the adhesion force of the phase change microcapsule on the textile substrate is strong.
Example 2
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: taking tetradecyl alcohol as a phase-change core material, CTAB as an emulsifying agent, taking water as a dispersion medium, starting high-speed emulsification for 30min, taking out, pouring into a 500ml three-neck flask, adding ammonia water, setting a constant-temperature reaction condition at 40 ℃, adding ethyl orthosilicate and ethanol into the reaction flask, setting a stirring rate of 260r/min, taking out after stirring for 24h, and obtaining the phase-change microcapsule taking silicon dioxide as a shell layer.
(2) Modification of phase-change microcapsules: taking 100g of prepared nano phase-change microcapsule emulsion, performing ultrasonic dispersion for 15min, adding 10g of vinyl trimethoxy silane which is subjected to ultrasonic prehydrolysis for 20min in 40 parts of water, placing the mixed solution in a reaction kettle at 80 ℃, setting the stirring speed of 400r/min, discharging after reacting for 5h, and filtering to obtain the modified phase-change microcapsule emulsion.
(3) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm (length. Times. Width) of polyester fabric, 100g of hydroxyethyl acrylate dispersion medium, 15g of modified phase change microcapsule emulsion and 1g of ultraviolet initiator 2-hydroxy-2-methyl-1-phenyl-1-acetone.
(4) Preparing a heat-accumulating temperature-regulating textile: and ultrasonically dispersing the mixed solution consisting of the hydroxyethyl acrylate dispersion medium, the modified phase-change microcapsule emulsion and the ultraviolet initiator 2-hydroxy-2-methyl-1-phenyl-1-acetone for 15min, then applying the mixed solution to the surface of the polyester fabric, vertically clamping the polyester fabric with the reaction solution applied by using two transparent glass plates, irradiating for 1.5min under a 250W ultraviolet high-pressure mercury lamp, and taking out the treated cotton fabric to obtain the phase-change microcapsule heat-accumulating temperature-regulating textile.
The phase-change microcapsule heat-accumulating temperature-regulating textile obtained in example 2 was subjected to a water washing test, and the test method was the same as in example 1.
Through detection, the obtained phase-change microcapsule has smooth surface, the phase-change latent heat value is 70J/g, the weight gain of the heat-storage temperature-regulating polyester fabric is 20.8%, the melting phase-change temperature is 38.6 ℃, the phase-change latent heat is 14.3J/g, and the reactive phase-change microcapsule is obviously attached to the polyester fabric after ultraviolet light solidification. After washing for 10 times, the weight gain of the heat accumulating and temperature regulating polyester fabric is 20.1%, and the phase transition latent heat is 13.9J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are not changed greatly after the textile is subjected to comparative washing for 10 times, which indicates that the adhesion force of the phase change microcapsule on the textile substrate is strong.
Example 3
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: the phase-change microcapsule taking silicon dioxide as a shell layer is prepared by taking dodecanol as a phase-change core material, taking CTAB as an emulsifying agent, taking out water as a dispersing medium, starting high-speed emulsification for 30min, taking out, pouring into a 500ml three-neck flask, adding ammonia water, setting a constant-temperature reaction condition at 40 ℃, adding ethyl orthosilicate and ethanol into the reaction flask, setting a stirring rate of 260r/min, taking out after stirring for 24h, and obtaining the phase-change microcapsule taking silicon dioxide as the shell layer.
(2) Modification of phase-change microcapsules: taking 100g of prepared nano phase-change microcapsule emulsion, performing ultrasonic dispersion for 15min, adding 10g of gamma- (methacryloyloxy) propyl trimethoxysilane which is subjected to ultrasonic prehydrolysis for 20min in 40 parts of water, placing the mixed solution in a reaction kettle at 80 ℃, setting the stirring speed of 350r/min, discharging after the reaction is performed for 3h, and filtering to obtain the modified phase-change microcapsule emulsion.
(3) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm x 10cm (length x width), 100g of hydroxyethyl acrylate dispersion medium, 5g of modified phase-change microcapsule emulsion and 0.5g of ultraviolet initiator azodiisobutyronitrile.
(4) Preparing a heat-accumulating temperature-regulating textile: and (3) ultrasonically dispersing the mixed solution consisting of the hydroxyethyl acrylate dispersion medium, the modified phase-change microcapsule emulsion and the ultraviolet initiator azodiisobutyronitrile for 15min, then applying the mixed solution to the surface of the silk fabric, vertically clamping the silk fabric with the reaction solution applied by using two transparent glass plates, irradiating for 1min under a 250W ultraviolet high-pressure mercury lamp, and taking out the treated silk fabric to obtain the phase-change microcapsule heat-storage temperature-regulating textile.
The phase-change microcapsule heat-accumulating temperature-regulating textile obtained in example 3 was subjected to a water washing test, and the test method was the same as in example 1.
Through detection, the obtained phase-change microcapsule has smooth surface, the phase-change latent heat value is 70J/g, the weight gain of the heat-storage temperature-regulating silk fabric is 24.9%, the melting phase-change temperature is 22.6 ℃, the phase-change latent heat is 17.1J/g, and the reactive phase-change microcapsule is obviously attached to the silk fabric after ultraviolet light solidification. After washing for 10 times, the weight gain of the heat-accumulating temperature-regulating real silk fabric is 24.1%, and the phase change latent heat is 16.7J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are not changed greatly after the textile is subjected to comparative washing for 10 times, which indicates that the adhesion force of the phase change microcapsule on the textile substrate is strong.
Example 4
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: taking tetradecyl alcohol as a phase-change core material, CTAB as an emulsifying agent, taking water as a dispersion medium, starting high-speed emulsification for 30min, taking out, pouring into a 500ml three-neck flask, adding ammonia water, setting a constant-temperature reaction condition at 40 ℃, adding ethyl orthosilicate and ethanol into the reaction flask, setting a stirring rate of 260r/min, taking out after stirring for 24h, and obtaining the phase-change microcapsule taking silicon dioxide as a shell layer.
(2) Modification of phase-change microcapsules: taking 100g of prepared nano phase-change microcapsule emulsion, performing ultrasonic dispersion for 15min, adding 15g of triethoxyvinyl which is subjected to ultrasonic prehydrolysis for 25min in 40 parts of water, placing the mixed solution in a reaction kettle at 75 ℃, setting the stirring speed of 350r/min, discharging after 4h of reaction, and filtering to obtain the modified phase-change microcapsule emulsion.
(3) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm by 10cm (length by width), 100g of hydroxypropyl acrylate dispersion medium, 12g of modified phase change microcapsule emulsion, and 0.75g of blue photoinitiator camphorquinone.
(4) Preparing a heat-accumulating temperature-regulating textile: and (3) ultrasonically dispersing the mixed solution consisting of the hydroxypropyl acrylate dispersion medium, the modified phase-change microcapsule emulsion and the blue photoinitiator camphorquinone for 15min, then applying the mixed solution to the surface of the nylon fabric, vertically clamping the nylon fabric with the reaction solution applied by using two transparent glass plates, irradiating for 5min under a blue light LED lamp of 200W, and taking out the treated nylon fabric to obtain the phase-change microcapsule heat-storage temperature-regulating textile.
The phase-change microcapsule heat-accumulating temperature-regulating textile obtained in example 4 was subjected to a water washing test, and the test method was the same as in example 1.
Through detection, the obtained phase-change microcapsule has a smooth surface, a phase-change latent heat value of 85J/g, a heat-storage temperature-regulating nylon fabric weight gain of 19.7%, a melting phase-change temperature of 38.9 ℃ and a phase-change latent heat of 16.1J/g, and after blue light solidification, the reactive phase-change microcapsule is obviously attached to the nylon fabric. After washing for 10 times, the weight gain of the heat accumulating and temperature regulating nylon fabric is 19.2%, and the phase transition latent heat is 16.0J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are not changed greatly after the textile is subjected to comparative washing for 10 times, which indicates that the adhesion force of the phase change microcapsule on the textile substrate is strong.
Example 5
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: taking a mixture eutectic of lunar silicic acid and stearic acid as a phase-change core material, taking CTAB as an emulsifying agent, taking water as a dispersing medium, starting high-speed emulsification for 30min, taking out, pouring into a 500ml three-neck flask, adding ammonia water, setting a constant-temperature reaction condition at 40 ℃, adding ethyl orthosilicate and ethanol into the reaction flask, setting a stirring rate of 260r/min, taking out after stirring for 24h, and obtaining the phase-change microcapsule taking silicon dioxide as a shell layer.
(2) Modification of phase-change microcapsules: taking 100g of prepared nano phase-change microcapsule emulsion, performing ultrasonic dispersion for 15min, adding 10g of vinyl tri (b-methoxyethoxy) silane which is subjected to ultrasonic prehydrolysis for 25min in 40 parts of water, placing the mixed solution in a reaction kettle at 75 ℃, setting the stirring speed of 350r/min, discharging after reacting for 4h, and filtering to obtain the modified phase-change microcapsule emulsion.
(3) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm x 10cm (length x width), 100g of hydroxyethyl acrylate dispersion medium, 12g of modified phase-change microcapsule emulsion and 0.8g of ultraviolet initiator azodiisobutyronitrile.
(4) Preparing a heat-accumulating temperature-regulating textile: and (3) ultrasonically dispersing the mixed solution consisting of the hydroxyethyl acrylate dispersion medium, the modified phase-change microcapsule emulsion and the ultraviolet initiator azodiisobutyronitrile for 15min, then applying the mixed solution to the surface of the polyester-cotton fabric, vertically clamping the real silk fabric with the reaction solution applied by using two transparent glass plates, irradiating the real silk fabric for 2min under a high-voltage ultraviolet mercury lamp with the power of 250W, and taking out the treated polyester-cotton fabric to obtain the phase-change microcapsule heat-storage temperature-regulating textile.
The phase-change microcapsule heat-accumulating temperature-regulating textile obtained in example 5 was subjected to a water washing test, and the test method was the same as in example 1.
Through detection, the obtained phase-change microcapsule has smooth surface, the phase-change latent heat value is 60J/g, the weight gain of the heat-storage temperature-regulating polyester-cotton fabric is 21.6%, the melting phase-change temperature is 33.6 ℃, the phase-change latent heat is 12.2J/g, and after ultraviolet light curing, the reactive phase-change microcapsule is obviously attached to the polyester-cotton fabric. After washing for 10 times, the weight gain of the heat-accumulating temperature-regulating polyester-cotton fabric is 21.2%, and the phase change latent heat is 12.1J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are not changed greatly after the textile is subjected to comparative washing for 10 times, which indicates that the adhesion force of the phase change microcapsule on the textile substrate is strong.
Example 6
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: taking a mixture eutectic of lunar silicic acid, stearic acid and palmitic acid as a phase-change core material, taking CTAB as an emulsifying agent, taking water as a dispersing medium, starting high-speed emulsification for 30min, taking out, pouring into a 500ml three-neck flask, adding ammonia water, setting a constant-temperature reaction condition of 40 ℃, adding ethyl orthosilicate and ethanol into the reaction flask, setting a stirring rate of 260r/min, taking out after stirring for 24h, and obtaining the phase-change microcapsule taking silicon dioxide as a shell layer.
(2) Modification of phase-change microcapsules: taking 100g of prepared nano phase-change microcapsule emulsion, performing ultrasonic dispersion for 15min, adding 10g of vinyl tri (b-methoxyethoxy) silane which is subjected to ultrasonic prehydrolysis for 20min in 40 parts of water, placing the mixed solution in a reaction kettle at 75 ℃, setting the stirring speed of 350r/min, discharging after reacting for 5h, and filtering to obtain the modified phase-change microcapsule emulsion.
(3) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm x 10cm (length x width), 100g of hydroxypropyl acrylate dispersion medium, 5g of modified phase change microcapsule emulsion and 0.5g of ultraviolet light initiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide.
(4) Preparing a heat-accumulating temperature-regulating textile: and ultrasonically dispersing the mixed solution consisting of the hydroxypropyl acrylate dispersion medium, the modified phase-change microcapsule emulsion and the ultraviolet initiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide for 15min, then applying the mixed solution to the surface of the linen, vertically clamping the linen with the reaction solution by using two transparent glass plates, irradiating for 1min under a 250W ultraviolet high-pressure mercury lamp, and taking out the treated linen to obtain the phase-change microcapsule heat-storage temperature-regulating textile.
The phase-change microcapsule heat-accumulating temperature-regulating textile obtained in example 6 was subjected to a water washing test, and the test method was the same as in example 1.
Through detection, the obtained phase-change microcapsule has smooth surface, the phase-change latent heat value is 60J/g, the weight gain of the heat-storage temperature-regulating linen fabric is 17.9%, the melting phase-change temperature is 32.7 ℃, the phase-change latent heat is 10.1J/g, and the reactive phase-change microcapsule is obviously attached to the linen fabric after ultraviolet light solidification. After washing for 10 times, the weight gain of the heat accumulating and temperature regulating linen fabric is 17.5%, and the phase transition latent heat is 9.9J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are not changed greatly after the textile is subjected to comparative washing for 10 times, which indicates that the adhesion force of the phase change microcapsule on the textile substrate is strong.
Example 7
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: taking paraffin as a phase-change core material, taking CTAB as an emulsifying agent, taking water as a dispersion medium, starting high-speed emulsification for 30min, taking out, pouring into a 500ml three-neck flask, adding ammonia water, setting a constant-temperature reaction condition at 40 ℃, adding ethyl orthosilicate and ethanol into the reaction flask, setting a stirring rate of 260r/min, taking out of the flask after stirring for 24h, and obtaining the phase-change microcapsule taking silicon dioxide as a shell layer.
(2) Modification of phase-change microcapsules: taking 100g of prepared nano phase-change microcapsule emulsion, performing ultrasonic dispersion for 15min, adding 10g of gamma- (methacryloyloxy) propyl trimethoxysilane which is subjected to ultrasonic prehydrolysis in 40 parts of water for 15min, placing the mixed solution in a reaction kettle at 75 ℃, setting the stirring speed of 200r/min, discharging after reacting for 5h, and filtering to obtain the modified phase-change microcapsule emulsion.
(3) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm x 10cm (length x width), 100g of hydroxyethyl acrylate dispersion medium, 10g of modified phase change microcapsule emulsion, and 0.5g of blue photoinitiator 4-dimethylaminobenzoic acid ethyl ester.
(4) Preparing a heat-accumulating temperature-regulating textile: and ultrasonically dispersing the mixed solution consisting of the hydroxyethyl acrylate dispersion medium, the modified phase-change microcapsule emulsion and the blue light initiating agent 4-dimethylaminoethyl benzoate for 15min, then applying the mixed solution to the surface of the tencel fabric, clamping the silk fabric with the reaction solution applied by two transparent glass plates up and down, irradiating for 4.5min under a 200W blue light LED lamp, and taking out the treated tencel fabric to obtain the phase-change microcapsule heat-storage temperature-regulating textile.
The phase-change microcapsule heat-accumulating temperature-regulating textile obtained in example 7 was subjected to a water washing test, and the test method was the same as in example 1.
Through detection, the obtained phase-change microcapsule has smooth surface, the phase-change latent heat value is 99.8J/g, the weight gain of the heat-storage temperature-regulating tencel fabric is 15.6%, the melting phase-change temperature is 28.9 ℃, the phase-change latent heat is 14.7J/g, and after blue light solidification, the reactive phase-change microcapsule is obviously attached to the tencel fabric. After washing for 10 times, the weight gain of the heat-accumulating temperature-regulating tencel fabric is 15.2%, and the phase change latent heat is 14.5J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are not changed greatly after the textile is subjected to comparative washing for 10 times, which indicates that the adhesion force of the phase change microcapsule on the textile substrate is strong.
Example 8
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: taking paraffin as a phase-change core material, taking CTAB as an emulsifying agent, taking water as a dispersion medium, starting high-speed emulsification for 30min, taking out, pouring into a 500ml three-neck flask, adding ammonia water, setting a constant-temperature reaction condition at 40 ℃, adding ethyl orthosilicate and ethanol into the reaction flask, setting a stirring rate of 260r/min, taking out of the flask after stirring for 24h, and obtaining the phase-change microcapsule taking silicon dioxide as a shell layer.
(2) Modification of phase-change microcapsules: taking 100g of prepared nano phase-change microcapsule emulsion, performing ultrasonic dispersion for 15min, adding 10g of gamma- (methacryloyloxy) propyl trimethoxysilane which is subjected to ultrasonic prehydrolysis for 20min in 40 parts of water, placing the mixed solution in a reaction kettle at 75 ℃, setting the stirring speed of 200r/min, discharging after reacting for 5h, and filtering to obtain the modified phase-change microcapsule emulsion.
(3) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm x 10cm (length x width) of modal fabric, 100g of hydroxyethyl acrylate dispersion medium, 10g of modified phase change microcapsule emulsion, 0.5g of blue photoinitiator camphorquinone.
(4) Preparing a heat-accumulating temperature-regulating textile: and (3) ultrasonically dispersing the mixed solution consisting of the hydroxyethyl acrylate dispersion medium, the modified phase-change microcapsule emulsion and the blue photoinitiator camphorquinone for 15min, then applying the mixed solution to the surface of a modal fabric, vertically clamping the real silk fabric with the reaction solution applied by using two transparent glass plates, irradiating for 5min under a 200W blue light LED lamp, and taking out the treated modal fabric to obtain the phase-change microcapsule heat-storage temperature-regulating textile.
The phase-change microcapsule heat-accumulating temperature-regulating textile obtained in example 8 was subjected to a water washing test, and the test method was the same as in example 1.
Through detection, the obtained phase-change microcapsule has smooth surface, the phase-change latent heat value is 98.5J/g, the weight gain of a heat accumulating fabric of Wen Mo is 19.1%, the melting phase-change temperature is 28.6 ℃, the phase-change latent heat is 18.2J/g, and after blue light solidification, the reactive phase-change microcapsule is obviously attached to a modal fabric. After washing for 10 times, the weight gain of the heat-accumulating temperature-regulating modal fabric is 18.8%, and the phase transition latent heat is 18.0J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are not changed greatly after the textile is subjected to comparative washing for 10 times, which indicates that the adhesion force of the phase change microcapsule on the textile substrate is strong.
Comparative example 1
A preparation method of a heat-accumulating temperature-regulating textile comprises the following steps:
(1) Preparation of phase-change microcapsules: as described in example 1.
(2) Raw material preparation of heat-accumulating temperature-regulating textiles: 10cm x 10cm (length x width), 100g of hydroxyethyl acrylate dispersion medium, 5g of phase-change microcapsule emulsion and 0.5g of ultraviolet initiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide.
(3) Preparing a heat-accumulating temperature-regulating textile: and ultrasonically dispersing the mixed solution consisting of the hydroxyethyl acrylate dispersion medium, the phase-change microcapsule emulsion and the ultraviolet initiator 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide for 15min, then applying the mixed solution to the surface of pure cotton fabric, vertically clamping the cotton fabric with the reaction solution by using two transparent glass plates, irradiating for 1min under a 250W ultraviolet high-pressure mercury lamp, and taking out the treated cotton fabric to obtain the phase-change microcapsule heat-storage temperature-regulating textile.
The phase-change microcapsule heat-accumulating temperature-regulating textile obtained in this comparative example was subjected to a water washing test, and the test method was the same as in example 1.
Through detection, the obtained phase-change microcapsule has a smooth surface, a phase-change latent heat value of 110J/g, a heat-storage temperature-regulating cotton fabric weight gain of 28.5%, a melting phase-change temperature of 27.8 ℃ and a phase-change latent heat of 30.4J/g, and after ultraviolet light curing, the reactive phase-change microcapsule is obviously attached to the cotton fabric. After washing for 10 times, the weight gain of the heat accumulating and temperature regulating cotton fabric is 20.3%, and the phase transition latent heat is 22.1J/g. The weight gain rate and the phase change latent heat of the heat-accumulating temperature-regulating textile are greatly changed after the textile is subjected to comparative washing for 10 times, and the phase change microcapsule is seriously stripped on the textile substrate, so that the unmodified phase change microcapsule can not be stably and firmly attached to the surface of the textile substrate by the aid of the adhesive hydroxyethyl acrylate.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The heat-accumulating temperature-regulating textile is characterized in that the heat-accumulating temperature-regulating textile is prepared by coating a mixture consisting of modified phase-change microcapsules, an organic monomer dispersion medium and an initiator on the surface of a textile substrate to form a coating, wherein the modified phase-change microcapsules are prepared by modifying phase-change microcapsules taking silicon dioxide as a shell layer and a phase-change material as a core material by a silane coupling agent;
the phase change material is any one of paraffin, fatty acid and fatty alcohol or a mixture eutectic of any two or more of the paraffin, fatty acid and fatty alcohol, wherein the phase change temperature of the phase change material is 22-40 ℃;
the organic monomer dispersion medium is any one of hydroxyethyl acrylate and hydroxypropyl acrylate;
the silane coupling agent is any one of gamma- (methacryloxy) propyl trimethoxy silane, vinyl trimethoxy silane, triethoxy vinyl and vinyl tri (b-methoxyethoxy) silane;
the initiator is a photoinitiator, including an ultraviolet initiator or a blue photoinitiator.
2. The heat and temperature regulating textile product according to claim 1, wherein the ultraviolet light initiator is any one of 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-propanone and azobisisobutyronitrile.
3. The heat and temperature regulating textile of claim 1, wherein the blue photoinitiator is any one of 1-phenyl-1, 2-propanedione and ethyl 4- (dimethylamino) benzoate.
4. The heat and temperature accumulating textile according to claim 1, wherein the textile substrate is any one of cotton, silk, polyester cotton, modal, tencel, polypropylene nonwoven and polyester nonwoven.
5. A method for preparing a heat accumulating and temperature regulating textile product according to claim 1, comprising the steps of:
(1) Preparation of modified phase-change microcapsules: ultrasonically dispersing phase-change microcapsule emulsion taking silicon dioxide as a shell layer and a phase-change material as a core material for 15min, adding a silane coupling agent which accounts for 10-15% of the mass of the phase-change microcapsule emulsion and is pre-hydrolyzed, placing the obtained mixed solution into a reaction kettle at 70-80 ℃, reacting for 3-6 h at a stirring speed of 200-300 r/min, discharging, and filtering to obtain the modified phase-change microcapsule;
(2) Preparing a heat-accumulating temperature-regulating textile: and (3) performing ultrasonic dispersion on a mixed solution consisting of an organic monomer dispersion medium, a modified phase-change microcapsule emulsion and an initiator for 15min, coating the mixed solution on the surface of a textile substrate, and performing curing treatment to obtain the heat-accumulating temperature-regulating textile.
6. The method according to claim 5, wherein the initiator in the step (2) is a photoinitiator, and the curing treatment is a curing treatment under irradiation of a light source for 1 to 5 minutes.
7. The method of claim 6, wherein the light source is an ultraviolet high pressure mercury lamp with a center wavelength at 365nm at a power of 250W or a blue LED lamp with a center wavelength at 425nm at a power of 200W.
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| CN112552878A (en) * | 2020-10-28 | 2021-03-26 | 杭州乐铭科技有限公司 | Phase change microcapsule, phase change microcapsule fiber and preparation method thereof |
| CN113278277A (en) * | 2021-05-25 | 2021-08-20 | 江苏晨光涂料有限公司 | Hybrid shell microcapsule-polyurethane phase change composite material |
| CN113417147A (en) * | 2021-06-29 | 2021-09-21 | 上海护理佳实业有限公司 | Intelligent temperature-adjusting non-woven fabric and absorbent product |
| CN113403853A (en) * | 2021-07-29 | 2021-09-17 | 东台市东驰服装有限公司 | Waterproof and moisture permeable radiation-proof fabric and preparation method thereof |
| CN116463106B (en) * | 2023-03-30 | 2023-09-29 | 杭州尚选科技有限公司 | Phase-change temperature-regulating microcapsule for textile and preparation method thereof |
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