CN106758264A - A kind of preparation method of temperature-regulating fiber, temperature-regulating fiber and thermostat quilt - Google Patents
A kind of preparation method of temperature-regulating fiber, temperature-regulating fiber and thermostat quilt Download PDFInfo
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- CN106758264A CN106758264A CN201611005102.8A CN201611005102A CN106758264A CN 106758264 A CN106758264 A CN 106758264A CN 201611005102 A CN201611005102 A CN 201611005102A CN 106758264 A CN106758264 A CN 106758264A
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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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- A—HUMAN NECESSITIES
- A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
- A47G—HOUSEHOLD OR TABLE EQUIPMENT
- A47G9/00—Bed-covers; Counterpanes; Travelling rugs; Sleeping rugs; Sleeping bags; Pillows
- A47G9/02—Bed linen; Blankets; Counterpanes
- A47G9/0207—Blankets; Duvets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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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
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
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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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
- D06M15/233—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated aromatic, e.g. styrene
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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
- D06M2101/02—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
- 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
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
- D06M2101/08—Esters or ethers of cellulose
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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
- D06M2101/12—Keratin fibres 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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- 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
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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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
- D06M2101/32—Polyesters
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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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Abstract
The temperature-regulating fiber made the present invention relates to functional fiber and its product technique field, the preparation method of specifically a kind of temperature-regulating fiber and of the method, further relates to the quilt made of the temperature-regulating fiber.The preparation method of temperature-regulating fiber is comprised the following steps：(1) raw material prepares；(2) prepared by oil phase component；(3) prepared by water phase components；(4) emulsifying raw material；(5) monomer polymerization.It is last that fiber is padded into 10 30min in the phase-change microcapsule emulsion for obtaining under conditions of 80 DEG C, then dried at 80 100 DEG C, temperature-regulating fiber is obtained.The present invention is based on phase-change microcapsule technology, and by the phase-change microcapsule of latent heat high, little particle and good stability by special process treatment on fiber, obtained temperature-regulating fiber has that temperature adjustment is uniform, latent heat is high and the comfortable advantage of body-sensing.
Description
Technical field
The present invention relates to functional fiber and its product technique field, specifically a kind of preparation method of temperature-regulating fiber with
And the temperature-regulating fiber made of the method, further relate to the thermostat quilt made of the temperature-regulating fiber.
Background technology
Scientific investigations showed that, 32 DEG C of quilt is favorably improved the sleep quality of people, at this temperature people be easiest into
Sleep.Because the skin temperature of people is lower than body temperature 5 DEG C, about 32 DEG C or so, quilt temperature is low, it is necessary to be warmed up with body temperature for a long time
Heat, not only expends the heat energy of human body, and after body surface undergoes the cold stimulation of a period of time, cerebral cortex can be made excited, so that
People's time for falling asleep is postponed, if quilt temperature is higher than 32 DEG C, human body is same because feeling that too hot needs perspire cooling, so as to reduce
Sleep quality.
Intelligent thermoregulating, using the temperature of temperature adjustment heat accumulating phase change material regulation control quilt, makes it permanent by based on above-mentioned phenomenon
32 DEG C or so are scheduled on, so as to help to maintain nice and cool, comfortable healthy sleep environment.Intelligent thermoregulating is usually by with temperature adjustment
Functional material is made, and play temperature adjustment function is phase-change material (PCM) of the addition in quilt.PCM materials in intelligent thermoregulating cloth
Material can absorb, store and discharge heat, can be warmed with heat release when temperature is low with absorbing and cooling temperature when temperature is high, so as to play
Temperature adjustment is acted on.
The utility model patent of such as Publication No. CN105411301A discloses a kind of self-temperature-regulating quilt, including by sublist
The filler filled in face and quilt surface, quilt surface is viscose rayon and the Outlast acrylic fibers containing phase-change material
Blending into fabric, filler material is PFY and the Outlast acrylic fiber blending containing phase-change material, is filled out
Fill fibres and use concaveconvex structure.
Additionally, the utility model patent of Publication No. CN201248559Y discloses a kind of Intelligent temperature regulating bedding article, by
Wadding part composition is cased with outer cover or outer cover, the outer cover is docked by common textile fabric with the temperature adjustment weaving face fabric with phase-change material
Bilayer is sewn into form；It is described wadding part be made up of the temperature-regulating fiber with phase-change material or by commonly wad a quilt with cotton part layer with phase-change material
Temperature-regulating fiber layer is compound or mixes.Make band phase-change material using the fabric with phase-change material or wadding part on articles for use in bed
Fabric or wadding part portions proximate human body, by the conversion process of phase-change material solid-liquid at different temperatures heat absorption or
The phenomenon of heat release is adjusted realizing the comfort level to human body temperature.
Although above-mentioned patent is provided with certain thermoregulation effect, the addition manner of phase-change material and the shape in quilt
State determines the temperature adjustment function quality of product.Due to adding that phase-change material difficulty is big in non-woven fabrics, phase-change material in the product
Attachment stability is poor, and addition is relatively low, thus results in that finished product thermostat quilt thermoregulation effect is poor, and human feeling is not obvious, in addition phase transformation
The latent heat of material cannot meet the heat exchange demand of bedding in many cases.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of preparation method of temperature-regulating fiber, comprise the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 80-120 parts of phase transformation
Material, 20-40 part of styrene, 15-25 parts of methyl methacrylate, 3-7 parts of acrylic acid, 0.5-1.5 parts of silane idol
Connection agent, 0.4-0.6 parts of azodiisobutyronitrile, 3-7 parts of neopelex and 500-700 parts of water, the phase transformation
The phase transition temperature of material is 30-35 DEG C；
(2) prepared by oil phase component：By the phase-change material of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silicon
Alkane coupling agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30~45 DEG C；
(3) prepared by water phase components：The dodecyl sodium sulfate and deionized water of aforementioned proportion are stirred into work at 30-45 DEG C
Change, water phase components are obtained；
(4) emulsifying raw material：At a temperature of 30-45 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 5000-12000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5-20 hours at 80 DEG C, occurred poly-
Reaction is closed, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80-100 DEG C, temperature-regulating fiber is obtained.
The present invention is based on phase-change microcapsule technology, and the phase-change microcapsule of latent heat high, nano particle and good stability is passed through
To on fiber, obtained temperature-regulating fiber has that temperature adjustment is uniform, latent heat is high and the comfortable advantage of body-sensing for special process treatment.
It should be noted that the particle diameter of phase-change microcapsule particle is substantially low obtained in the raw material proportioning and processing technology of uniqueness
In the like product of prior art, Nano grade is reached, the specific surface area of particle is very big, so that microcapsule granule and fibre
Physisorption between dimension is very strong, and in use, phase-change microcapsule particle will not be from the surface desorption of temperature-regulating fiber.
In addition, microcapsules are prepared and organically linked together with the preparation of temperature-regulating fiber by the manufacture craft in this programme,
Or else with the premise of obtaining microcapsules dry powder, be directly prepared by microcapsule granule emulsion, save processing step and
Energy resource consumption, and phase-change microcapsule is evenly distributed, and phenomenon uneven in temperature is caused in the absence of local cluster.
Further, raw material of the phase-change microcapsule emulsion including following parts by weight, 100 parts of phase-change material,
30 parts of styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of azo two are different
Butyronitrile, 5 parts of neopelex and 600 parts of water, the raw material proportioning of optimization can obtain that latent heat is higher, and particle is more
The small phase-change microcapsule of refinement.
Further, described phase-change material is capric acid, the phase transition temperature of capric acid between 30-35 DEG C, be human body compared with
Easily enter dormant environment temperature interval, and the chemical stability of the two is stronger, being not susceptible in manufacturing process
Change is learned, product quality is influenceed.
Further, prepared by water phase components, oil phase component and the temperature of emulsifying raw material is 37 DEG C, and this temperature is higher than phase transformation
The phase transition temperature of material, it is ensured that organic phase change material is in liquid, to be smoothed out emulsification, while drawing less than initiator again
Hair temperature, in order to avoid there is polymerisation before the emulsion of stabilization is formed.
Further, the rotating speed for being stirred during emulsifying raw material is 7500r/min, and ensure that makes oil phase in water phase
The dispersed emulsion droplet for forming appropriate diameter.
Further, the time heated in monomer is 10 hours, can fully ensure that Raolical polymerizable is complete
Into.
Further, the drying temperature in step 2 is 90 DEG C, it is ensured that the active group on capsule top layer fills with fiber surface
Divide bonding, enhancing and fiber adhesive force, so as to improve the stability of temperature-regulating fiber.
Additionally, the present invention also protects the temperature-regulating fiber being prepared from using above-mentioned preparation method accordingly.
Further, the mass fraction of the phase-change microcapsule for adhering on the temperature-regulating fiber is 10%~30%, its latent heat
It is worth between 15-50J/g, with obvious thermoregulation effect..
Additionally, the present invention also protects a kind of thermostat quilt, comprising core and the back side, the core is fine by above-described temperature adjustment
Dimension is made.
Beneficial effect of the present invention specifically show it is following some：
Based on phase-change microcapsule technology, the phase-change microcapsule of latent heat high, little particle and good stability is passed through into special process
Process on fiber, obtained temperature-regulating fiber has that temperature adjustment is uniform, latent heat is high and the comfortable advantage of body-sensing.Phase-change microcapsule can be
Even is attached to fiber surface, and capsule addition can be controlled in mass ratio 10%-30%, and fiber latent heat is up to latent heat up to 15-
50J/g.The phase-change microcapsule has nano-scale particle size, and high-hydrophilic can be with fiber strong bonded, rub resistance washing.
Brief description of the drawings
Fig. 1：The photo figure of the SEM of the phase-change microcapsule of an embodiment of the present invention.
Fig. 2：The photo figure of the SEM of the temperature-regulating fiber of an embodiment of the present invention.
Specific embodiment
Phase-change material has the ability for changing its physical state in certain temperature range.By taking solid-liquid phase change as an example, adding
When heat is to fusion temperature, the phase transformation from solid-state to liquid is just produced, during fusing, phase-change material absorbs and stores substantial amounts of
Latent heat；When phase-change material is cooled down, during the heat of storage will be dispersed into environment within the scope of certain temperature, carry out from liquid
To the reverse transformation of solid-state.In both phase transition process, stored or release energy is referred to as latent heat of phase change.Physical state occurs
During change, the temperature of material itself almost remains unchanged before phase transformation completion, forms a temperature platform wide, although temperature is not
Become, but the latent heat of absorption or release is quite big.
Using this kind of superior property of phase-change material, articles for use field, using phase-change material, phase-change material is implanted into bed
In fiber, can greatly change the quality of life of people, any energy is not used, quilt can be allowed to become micro- air-conditioning.
The present invention specifically provides the system that a kind of potential heat value that make use of phase-change material carries out the temperature-regulating fiber of temperature adjustment
Make method, comprise the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 80-120 parts of phase transformation
Material, 20-40 part of styrene, 15-25 parts of methyl methacrylate, 3-7 parts of acrylic acid, 0.5-1.5 parts of silane idol
Connection agent, 0.4-0.6 parts of azodiisobutyronitrile, 3-7 parts of neopelex and 500-700 parts of water, the phase transformation
The phase transition temperature of material is 30-35 DEG C.Wherein, phase-change material as phase-change microcapsule capsule-core, styrene, methyl methacrylate
Ester and acrylic acid, by there is polymerisation, form cyst wall as the reaction raw material of the cyst wall of phase-change microcapsule, eventually through
Cyst wall coats capsule-core, forms microcapsules shape.Wherein as the crosslinking agent of polymerisation, azodiisobutyronitrile does silane coupler
It is the initiator of polymerisation, neopelex is used as emulsifying agent.It should be noted that phase transformation material therein
The phase transition temperature of material is preferably between 30-35 DEG C, and the quilt that the temperature-regulating fiber produced is processed into can be convenient for people to fall asleep, excellent
Choosing uses capric acid；The reaction raw material of cyst wall are also not limited to three kinds of above-mentioned materials, can also be other monomers, such as
Methyl acrylate, ethyl acrylate, butyl acrylate, tert-butyl acrylate, Isooctyl acrylate monomer, divinylbenzene and dimethyl
Acrylic acid glycol ester etc.；Initiator can also be ABVN or azo-bis-iso-dimethyl；Emulsifying agent can be with
It is Tween-80 or Arlacel-80.
(2) prepared by oil phase component：By the phase-change material of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silicon
Alkane coupling agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30~45 DEG C；
(3) prepared by water phase components：The neopelex and deionized water of aforementioned proportion are stirred at 30-45 DEG C
Activation, is obtained water phase components；
(4) emulsifying raw material：At a temperature of 30-45 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 5000-12000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5-20 hours at 80 DEG C, occurred poly-
Reaction is closed, phase-change microcapsule emulsion is obtained.Nitrogen protection can prevent influence of the oxygen to polymerisation, and oxygen is too active,
Efficiency of initiation can be influenceed, more side reaction can be also increased in polymerization process.Certainly, protection gas can also use other indifferent gas
Body, such as helium or argon gas
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80-100 DEG C, temperature-regulating fiber is obtained.Wherein, described fiber can be animal and plant fiber, such as cotton, fiber crops, silk, sheep
Hair, cashmere etc.；Can be staple fibre, such as viscose rayon, CUP, acetate fiber；Synthetic fibers are can also be, it is such as poly-
The fibrous material of any one or its any combination in ester fiber, polyacrylonitrile fibre, Fypro etc..
The present invention is described in further detail below by specific embodiment.Phase-change microcapsule of the invention and
The surface topography of temperature-regulating fiber and the sign of performance use following equipment in addition to especially indicating：
It is micro- using the phase transformation after the drying of Jeol Ltd. JSM-5610LV types scanning electronic microscope observation, metal spraying
The surface topography of capsule.
Phase-change microcapsule is tested using Malvern Instr Ltd. of Britain Mastersizer 2000E types laser particle analyzer
Granularity.
Using platinum Ai Ermo Instrument Ltd. of U.S. Pyris DimondC types differential scanning calorimeter (DSC), in nitrogen
Under gas shielded, the DSC scanning curves of test 10 DEG C/min temperature-rise periods and -10 DEG C/min temperature-fall periods obtain phase-change material micro-
The latent heat of phase change of capsule.
Using Wenzhou Darong Textile Instrument Co., Ltd. YG-606E type fabric heat-insulation ability meters in national standard side
The insulation rate of temperature-regulating fiber is tested under method AATCC standard conditions.
The present invention does not address part and is applied to prior art.
Specific embodiment of the invention is given below：But specific embodiment is merely to be described in further detail this explanation,
It is not intended to limit claim of the invention.
Embodiment 1
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 80 parts of capric acid, 20
The styrene of part, 15 parts of methyl methacrylate, 3 parts of acrylic acid, 0.5 part of silane coupler, 0.4 part of azo two are different
Butyronitrile, 3 parts of neopelex and 500 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 30 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 30 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 500nm, and phase transition temperature is 31.5 DEG C, and latent heat of phase change is
136J/g。
The quality accounting of phase-change microcapsule is 10% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 13.6J/g, insulation
Rate is 81%.
The photo of the SEM of the phase-change microcapsule that above-described embodiment is obtained is as shown in figure 1, resulting tune
The photo of the SEM of warm fiber is as shown in Figure 2.
Embodiment 2
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 120 parts of capric acid, 40
The styrene of part, 25 parts of methyl methacrylate, 7 parts of acrylic acid, 1.5 parts of silane coupler, 0.6 part of azo two are different
Butyronitrile, 7 parts of neopelex and 700 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 30 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 30 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 650nm, and phase transition temperature is 32.3 DEG C, and latent heat of phase change is
143J/g。
The quality accounting of phase-change microcapsule is 20% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 28.6J/g, insulation
Rate is 84%.
Embodiment 3
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 30 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 30 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 800nm, and phase transition temperature is 32.1 DEG C, and latent heat of phase change is
148J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 44.4J/g, insulation
Rate is 85%.
Embodiment 4
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 110 parts of capric acid, 35
The styrene of part, 25 parts of methyl methacrylate, 6 parts of acrylic acid, 1.3 parts of silane coupler, 0.6 part of azo two are different
Butyronitrile, 6 parts of neopelex and 650 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 30 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 30 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 700nm, and phase transition temperature is 31.9 DEG C, and latent heat of phase change is
129J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 38.7J/g, insulation
Rate is 82%.
Embodiment 5
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 900nm, and phase transition temperature is 32.1 DEG C, and latent heat of phase change is
152J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 45.6J/g, insulation
Rate is 86%.
Embodiment 6
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 45 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 45 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 45 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 620nm, and phase transition temperature is 32.4 DEG C, and latent heat of phase change is
146J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 43.8J/g, insulation
Rate is 84%.
Embodiment 7
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 7500r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 400nm, and phase transition temperature is 31.8 DEG C, and latent heat of phase change is
159J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 47.7J/g, insulation
Rate is 84%.
Embodiment 8
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 220nm, and phase transition temperature is 32.0 DEG C, and latent heat of phase change is
162J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 48.6J/g, insulation
Rate is 86%.
Embodiment 9
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 12000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5 hours at 80 DEG C, polymerization occurs anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 190nm, and phase transition temperature is 32.2 DEG C, and latent heat of phase change is
168J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 50.4J/g, insulation
Rate is 87%.
Embodiment 10
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 10 hours at 80 DEG C, be polymerized
Reaction, is obtained phase-change microcapsule emulsion.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 200nm, and phase transition temperature is 32.3 DEG C, and latent heat of phase change is
153J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 45.9J/g, insulation
Rate is 84%.
Embodiment 11
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 15 hours at 80 DEG C, be polymerized
Reaction, is obtained phase-change microcapsule emulsion.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 310nm, and phase transition temperature is 31.8 DEG C, and latent heat of phase change is
149J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 44.7J/g, insulation
Rate is 86%.
Embodiment 12
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 20 hours at 80 DEG C, be polymerized
Reaction, is obtained phase-change microcapsule emulsion.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 80 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 260nm, and phase transition temperature is 32.1 DEG C, and latent heat of phase change is
157J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 47.1J/g, insulation
Rate is 87%.
Embodiment 13
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 10 hours at 80 DEG C, be polymerized
Reaction, is obtained phase-change microcapsule emulsion.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 90 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 340nm, and phase transition temperature is 32.4 DEG C, and latent heat of phase change is
139J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 41.7J/g, insulation
Rate is 88%.
Embodiment 14
A kind of preparation method of temperature-regulating fiber, comprises the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 100 parts of capric acid, 30
The styrene, 20 parts of methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupler, 0.5 part of the isobutyl of azo two of part
Nitrile, 5 parts of neopelex and 600 parts of water；
(2) prepared by oil phase component：By the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C；
(3) prepared by water phase components：By the dodecyl sodium sulfate and deionized water of aforementioned proportion at 37 DEG C stir-activating,
Water phase components are obtained；
(4) emulsifying raw material：At a temperature of 37 DEG C, the oil phase component is added in water phase components, and with
The rotating speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) monomer polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 10 hours at 80 DEG C, be polymerized
Reaction, is obtained phase-change microcapsule emulsion.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then
Dried at 100 DEG C, temperature-regulating fiber is obtained.
After testing, the average grain diameter of gained phase-change microcapsule is 230nm, and phase transition temperature is 31.9 DEG C, and latent heat of phase change is
143J/g。
The quality accounting of phase-change microcapsule is 30% in gained temperature-regulating fiber, and the latent heat of temperature-regulating fiber is 42.9J/g, insulation
Rate is 87%.
Test example：The phase-change microcapsule attachment uniformity testing of temperature-regulating fiber surface
Test material：Embodiment 10, embodiment 13 and temperature-regulating fiber, Publication No. obtained in embodiment 14
Temperature-regulating fiber obtained in the scheme that embodiment 3 described in the application for a patent for invention of CN104562258A is used, hereinafter referred to as
Reference examples.
Test method：The temperature-regulating fiber prepared by embodiment 10, embodiment 13, embodiment 14 and reference examples is randomly selected to fit
Amount, is respectively cut the segment for 3mm, and each embodiment randomly selects 10 sections of temperature-regulating fibers, using differential scanning calorimeter
(DSC) DSC scanning curves, under nitrogen protection, are drawn, every section of latent heat of phase change of temperature-regulating fiber is obtained.And remember result of the test
Record is in table 1.
By table 1, each portion of the temperature-regulating fiber prepared by embodiments of the invention 10, embodiment 13 and embodiment 14
The extreme value and standard deviation of the test result of potential heat value is divided all to be significantly lower than reference examples of the prior art, and the former test is equal
Value illustrates that the phase-change microcapsule particle on the temperature-regulating fiber obtained by technical scheme is distinguished very apparently higher than the latter
Uniformly, without significantly assembling or adhere to blind area, and potential heat value apparently higher than like product of the prior art.
The temperature-regulating fiber surface phase-change microcapsule of table 1 adheres to uniformity testing result (J/g)
| Testing time | Embodiment 10 | Embodiment 13 | Embodiment 14 | Reference examples |
| 1 | 46.2 | 40.9 | 43.3 | 18.3 |
| 2 | 46.1 | 41.5 | 43.6 | 19.4 |
| 3 | 45.2 | 43.0 | 42.7 | 20.8 |
| 4 | 46.8 | 42.7 | 42.6 | 22.6 |
| 5 | 46.4 | 41.4 | 42.8 | 23.7 |
| 6 | 44.8 | 40.8 | 41.7 | 18.5 |
| 7 | 46.5 | 41.9 | 43.5 | 17.9 |
| 8 | 44.9 | 42.3 | 42.6 | 22.8 |
| 9 | 46.2 | 41.6 | 41.8 | 24.6 |
| 10 | 45.3 | 40.4 | 41.6 | 15.7 |
| Average | 45.84 | 41.65 | 42.62 | 20.43 |
| Extreme value | 2 | 2.6 | 2 | 8.9 |
| Standard deviation | 0.719877 | 0.839643 | 0.729992 | 2.918162 |
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of temperature-regulating fiber, it is characterised in that comprise the following steps：
Step one：The preparation of phase-change microcapsule emulsion
(1) raw material prepares：The phase-change microcapsule emulsion includes the raw material of following parts by weight, 80-120 parts of phase transformation material
Material, 20-40 parts of styrene, 15-25 parts of methyl methacrylate, 3-7 parts of acrylic acid, 0.5-1.5 parts silane coupled
Agent, 0.4-0.6 parts of azodiisobutyronitrile, 3-7 parts of neopelex and 500-700 parts of water, the phase transformation material
The phase transition temperature of material is 30-35 DEG C；
(2) prepared by oil phase component：By the phase-change material of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane idol
Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30~45 DEG C；
(3) prepared by water phase components：By the emulsifying agent and deionized water of aforementioned proportion at 30-45 DEG C stir-activating, water phase is obtained
Component；
(4) emulsifying raw material：At a temperature of 30-45 DEG C, the oil phase component is added in water phase components, and with 5000-
The rotating speed of 12000r/min is stirred emulsification, and homogeneous latex emulsion is obtained；
(5) emulsion polymerization：By above-mentioned homogeneous latex emulsion under nitrogen protection, heated 5-20 hours at 80 DEG C, trigger polymerization anti-
Should, phase-change microcapsule emulsion is obtained.
Step 2：Prepare temperature-regulating fiber
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule emulsion that step one is obtained, then in 80-
Dried at 100 DEG C, temperature-regulating fiber is obtained.
2. the preparation method of temperature-regulating fiber according to claim 1, it is characterised in that the phase-change microcapsule emulsion includes
The raw material of following parts by weight, 100 parts of phase-change material, 30 parts of styrene, 20 parts of methyl methacrylate, 5 parts
Acrylic acid, 1 part of silane coupler, 0.5 part of azodiisobutyronitrile, 5 parts of neopelex and 600 parts of water.
3. the preparation method of temperature-regulating fiber according to claim 1, it is characterised in that described phase-change material is capric acid.
4. the preparation method of temperature-regulating fiber according to claim 1, it is characterised in that prepared by water phase components, oil phase component
And the temperature of emulsifying raw material is 37 DEG C.
5. the preparation method of temperature-regulating fiber according to claim 1, it is characterised in that stirred during emulsifying raw material
Rotating speed is 7500r/min.
6. the preparation method of temperature-regulating fiber according to claim 1, it is characterised in that heated in emulsion polymerization process
Time is 10 hours.
7. the preparation method of temperature-regulating fiber according to claim 1, it is characterised in that the drying temperature in step 2 is 90
℃。
8. a kind of temperature-regulating fiber, it is characterised in that be prepared from using the preparation method described in any one of claim 1~7.
9. temperature-regulating fiber according to claim 8, it is characterised in that the phase-change microcapsule adhered on the temperature-regulating fiber
Mass fraction is 10%~30%.
10. a kind of thermostat quilt, comprising core and the back side, it is characterised in that temperature adjustment of the core as described in claim 8 or 9
Fiber is made.
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| CN107794770A (en) * | 2017-09-27 | 2018-03-13 | 浙江中科德商新材料股份有限公司 | A kind of method that uv-light polymerization in situ prepares temperature adjustment fabric |
| CN108998973A (en) * | 2018-08-10 | 2018-12-14 | 苏州市天翱特种织绣有限公司 | A kind of intelligent heat preserving fabric |
| CN111485428A (en) * | 2019-01-25 | 2020-08-04 | 浙江理工大学 | Heat-storage temperature-regulating textile and preparation method thereof |
| CN111721737A (en) * | 2020-06-15 | 2020-09-29 | 上海应用技术大学 | Characterization method for researching interaction mechanism of slow-release essence nanoparticles and paper |
| CN112127162A (en) * | 2020-09-16 | 2020-12-25 | 浙江中科微瑞新材料股份有限公司 | Intelligent microparticle treatment method for articles |
| CN113403704A (en) * | 2021-06-01 | 2021-09-17 | 深圳减字科技有限公司 | Preparation method of temperature-adjusting fiber, temperature-adjusting fiber and fabric |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029421A (en) * | 2007-04-17 | 2007-09-05 | 河北吉藁化纤有限责任公司 | Intelligent temperature-adjusting viscose fibre and its production |
| CN101824306A (en) * | 2010-03-23 | 2010-09-08 | 北京交通大学 | Method for preparing multi-phase change material coated with microcapsule |
| CN102676123A (en) * | 2012-04-10 | 2012-09-19 | 巢启 | Microcapsule preparation method of phase change material |
| CN102733192A (en) * | 2012-04-09 | 2012-10-17 | 福建众和股份有限公司 | Finishing technology of nano-grade phase-change microcapsule heat-accumulation temperature-adjustment intelligent textile fabric printed cloth |
| CN104117330A (en) * | 2014-08-08 | 2014-10-29 | 广西启利新材料科技股份有限公司 | Preparation method for twice coating of low-temperature phase change microcapsule |
-
2016
- 2016-11-15 CN CN201611005102.8A patent/CN106758264B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029421A (en) * | 2007-04-17 | 2007-09-05 | 河北吉藁化纤有限责任公司 | Intelligent temperature-adjusting viscose fibre and its production |
| CN101824306A (en) * | 2010-03-23 | 2010-09-08 | 北京交通大学 | Method for preparing multi-phase change material coated with microcapsule |
| CN102733192A (en) * | 2012-04-09 | 2012-10-17 | 福建众和股份有限公司 | Finishing technology of nano-grade phase-change microcapsule heat-accumulation temperature-adjustment intelligent textile fabric printed cloth |
| CN102676123A (en) * | 2012-04-10 | 2012-09-19 | 巢启 | Microcapsule preparation method of phase change material |
| CN104117330A (en) * | 2014-08-08 | 2014-10-29 | 广西启利新材料科技股份有限公司 | Preparation method for twice coating of low-temperature phase change microcapsule |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107794770A (en) * | 2017-09-27 | 2018-03-13 | 浙江中科德商新材料股份有限公司 | A kind of method that uv-light polymerization in situ prepares temperature adjustment fabric |
| CN107794770B (en) * | 2017-09-27 | 2022-05-03 | 浙江中科微瑞新材料股份有限公司 | Method for preparing temperature-adjusting fabric by in-situ ultraviolet light initiated polymerization |
| CN108998973A (en) * | 2018-08-10 | 2018-12-14 | 苏州市天翱特种织绣有限公司 | A kind of intelligent heat preserving fabric |
| CN111485428A (en) * | 2019-01-25 | 2020-08-04 | 浙江理工大学 | Heat-storage temperature-regulating textile and preparation method thereof |
| CN111485428B (en) * | 2019-01-25 | 2023-04-25 | 杭州尚选科技有限公司 | Heat-accumulating temperature-regulating textile and preparation method thereof |
| CN111721737A (en) * | 2020-06-15 | 2020-09-29 | 上海应用技术大学 | Characterization method for researching interaction mechanism of slow-release essence nanoparticles and paper |
| CN112127162A (en) * | 2020-09-16 | 2020-12-25 | 浙江中科微瑞新材料股份有限公司 | Intelligent microparticle treatment method for articles |
| CN113403704A (en) * | 2021-06-01 | 2021-09-17 | 深圳减字科技有限公司 | Preparation method of temperature-adjusting fiber, temperature-adjusting fiber and fabric |
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