CN106758264B - A kind of production method of temperature-regulating fiber, temperature-regulating fiber and thermostat quilt - Google Patents

A kind of production method of temperature-regulating fiber, temperature-regulating fiber and thermostat quilt Download PDF

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CN106758264B
CN106758264B CN201611005102.8A CN201611005102A CN106758264B CN 106758264 B CN106758264 B CN 106758264B CN 201611005102 A CN201611005102 A CN 201611005102A CN 106758264 B CN106758264 B CN 106758264B
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temperature
phase
parts
regulating fiber
change microcapsule
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CN106758264A (en
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张国庆
肖吕明
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Yiwu Yingke New Materials Technology Co.,Ltd.
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Zhejiang Yingfan New Mstar Technology Ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/12Processes in which the treating agent is incorporated in microcapsules
    • AHUMAN NECESSITIES
    • A47FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47GHOUSEHOLD OR TABLE EQUIPMENT
    • A47G9/00Bed-covers; Counterpanes; Travelling rugs; Sleeping rugs; Sleeping bags; Pillows
    • A47G9/02Bed linen; Blankets; Counterpanes
    • A47G9/0207Blankets; Duvets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/06Making microcapsules or microballoons by phase separation
    • B01J13/14Polymerisation; cross-linking
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00Copolymers 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
    • C08F212/02Monomers containing only one unsaturated aliphatic radical
    • C08F212/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06Hydrocarbons
    • C08F212/08Styrene
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188Monocarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/227Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
    • D06M15/233Macromolecular 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • D06M2101/08Esters or ethers of cellulose
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • D06M2101/12Keratin fibres or silk
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/18Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/26Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
    • D06M2101/28Acrylonitrile; Methacrylonitrile
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    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
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  • Polymers & Plastics (AREA)
  • Dispersion Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention relates to functional fiber and its product technique field, the production method of specifically a kind of temperature-regulating fiber and the temperature-regulating fiber made of this method further relate to the quilt made of the temperature-regulating fiber.The production method of temperature-regulating fiber is the following steps are included: (1) raw material preparation;(2) prepared by oil phase component;(3) prepared by water phase components;(4) emulsifying raw material;(5) monomer polymerization.Finally under conditions of 80 DEG C, fiber is padded into 10-30min in obtained phase-change microcapsule lotion, is then dried at 80-100 DEG C, temperature-regulating fiber is made.The present invention is based on phase-change microcapsule technologies, the good phase-change microcapsule of Gao Qianre, little particle and stability are handled by special process onto fiber, temperature-regulating fiber obtained has the advantages that temperature adjustment is uniform, latent heat is high and body-sensing is comfortable.

Description

A kind of production method of temperature-regulating fiber, temperature-regulating fiber and thermostat quilt
Technical field
The present invention relates to functional fiber and its product technique field, specifically a kind of production method of temperature-regulating fiber with And the temperature-regulating fiber made of this method, further relate to the thermostat quilt made of the temperature-regulating fiber.
Background technique
Scientific investigations showed that 32 DEG C of quilt helps to improve the sleep quality of people, at this temperature people be easiest into It sleeps.Because the skin temperature of people is 5 DEG C lower than body temperature, about 32 DEG C or so, quilt temperature is low, needs to be warmed up with body temperature for a long time After heat not only expends the thermal energy of human body, but also body surface is subjected to the cold stimulation of a period of time, cerebral cortex can be made excited, thus People's time for falling asleep is postponed, if quilt temperature is higher than 32 DEG C, human body is equally because feel that too hot needs perspire cooling, to reduce Sleep quality.
Intelligent thermoregulating is based on above-mentioned phenomenon, and the temperature of control quilt is adjusted using temperature adjustment heat accumulating phase change material, makes its perseverance 32 DEG C or so are scheduled on, 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 the phase-change material (PCM) added in quilt.PCM material in intelligent thermoregulating cloth Material can be absorbed, store and discharge heat, and temperature Gao Shike can be warmed with absorbing and cooling temperature when temperature is low with heat release, to play Temperature adjustment effect.
Such as the utility model patent of Publication No. CN105411301A discloses a kind of self-temperature-regulating quilt, including by sublist The filler filled in face and quilt surface, quilt surface are viscose rayon and the Outlast acrylic fiber containing phase-change material It is blended at fabric, filler material be polyester filament and Outlast acrylic fiber containing phase-change material it is blended made of, fill out Fibres are filled using concaveconvex structure.
In addition, the utility model patent of Publication No. CN201248559Y discloses a kind of Intelligent temperature regulating bedding article, by Wadding part composition is cased in outer cover or outer cover, the outer cover is docked by common textile fabric with the temperature adjustment textile fabric with phase-change material Bilayer is sewn into form;The wadding part be made 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 in bed Fabric or wadding part portions proximate human body, by the conversion process of the solid-liquid of phase-change material at different temperatures absorb heat or The phenomenon that heat release, to realize that the comfort level to human body temperature is adjusted.
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 added in non-woven fabrics phase-change material difficulty is big, phase-change material in the product Attachment stability is poor, and additive amount is lower, thus causes finished product thermostat quilt thermoregulation effect poor, and human feeling is unobvious, furthermore phase transformation The latent heat of material is unable to satisfy the heat exchange demand of bedding in many cases.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of production methods of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 80-120 parts of phase transformation Material, 20-40 parts of styrene, 15-25 parts of methyl methacrylate, 3-7 parts of acrylic acid, 0.5-1.5 parts of silane are even Join 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 of aforementioned proportion and deionized water are stirred to work at 30-45 DEG C Change, water phase components are made;
(4) emulsifying raw material: 30-45 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 5000-12000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5-20 hours at 80 DEG C, occurs poly- Reaction is closed, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80-100 DEG C, temperature-regulating fiber is made.
The present invention is based on phase-change microcapsule technologies, and the good phase-change microcapsule of Gao Qianre, nano particle and stability is passed through In special process processing to fiber, temperature-regulating fiber obtained has the advantages that temperature adjustment is uniform, latent heat is high and body-sensing is comfortable.
It should be noted that the partial size of phase-change microcapsule particle made from unique raw material proportioning and processing technology is obviously low In the similar product of the 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, the manufacture craft in this programme organically links together the preparation that microcapsules are prepared with temperature-regulating fiber, Or else under the premise of obtaining microcapsules dry powder, directly prepared by microcapsule granule lotion, save processing step and Energy consumption, and phase-change microcapsule is evenly distributed, and there is no local clusters to cause phenomenon uneven in temperature.
Further, the phase-change microcapsule lotion 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 of acrylic acid, 1 part of silane coupling agent, 0.5 part of azo two are different Butyronitrile, 5 parts of neopelex and 600 parts of water, the raw material proportioning of optimization, available latent heat is higher, and particle is more The small phase-change microcapsule of refinement.
Further, the 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 section, and the chemical stability of the two is stronger, being in the production process not susceptible to Variation is learned, product quality is influenced.
Further, the temperature of water phase components, oil phase component preparation and emulsifying raw material is 37 DEG C, this temperature is higher than phase transformation The phase transition temperature of material guarantees that organic phase change material is in liquid, to go on smoothly emulsification, while drawing lower than initiator again Temperature is sent out, in order to avoid polymerization reaction occurs before forming stable lotion.
Further, the revolving speed stirred during emulsifying raw material is 7500r/min, can guarantee to make oily phase in water phase The evenly dispersed emulsion droplet for forming appropriate diameter.
Further, the time heated in monomer is 10 hours, can fully ensure that Raolical polymerizable is complete At.
Further, the drying temperature in step 2 is 90 DEG C, guarantees that the active group on capsule surface layer is filled with fiber surface Divide bonding, enhancing and fiber adhesive force, to improve the stability of temperature-regulating fiber.
In addition, the temperature-regulating fiber that the also corresponding protection of the present invention is prepared using above-mentioned production method.
Further, the mass fraction of the phase-change microcapsule adhered on the temperature-regulating fiber is 10%~30%, latent heat Value has apparent thermoregulation effect between 15-50J/g.
In addition, the present invention also protects a kind of thermostat quilt, it include core and the back side, the core is fine by above-described temperature adjustment Dimension is made.
Beneficial effect of the present invention specifically shows the following:
Based on phase-change microcapsule technology, the good phase-change microcapsule of Gao Qianre, little particle and stability is passed through into special process It handles on fiber, temperature-regulating fiber obtained has the advantages that temperature adjustment is uniform, latent heat is high and body-sensing is comfortable.Phase-change microcapsule can be Even is attached to fiber surface, and capsule additive amount 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 firmly combined with fiber, rub resistance washing.
Detailed description of the invention
Fig. 1: the photo figure of the scanning electron microscope of the phase-change microcapsule of an embodiment of the present invention.
Fig. 2: the photo figure of the scanning electron microscope 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 arrives fusion temperature, the phase transformation from solid-state to liquid is just generated, during fusing, phase-change material is absorbed and stored a large amount of Latent heat;When phase-change material is cooling, the heat of storage will be dispersed into environment within the scope of certain temperature, be carried out from liquid To solid reverse transformation.In both phase transition process, stored or release energy is known as latent heat of phase change.Physical state occurs When variation, the temperature of material itself almost remains unchanged before phase transformation is completed, and a wide temperature platform is formed, although temperature is not Become, but the latent heat for absorbing or discharging is quite big.
Using such superior property of phase-change material, phase-change material is implanted by articles field using phase-change material in bed It in fiber, can greatly change people's lives quality, not use any energy, quilt can be allowed to become micro- air-conditioning.
The present invention specifically provides a kind of system of the temperature-regulating fiber of potential heat value progress temperature adjusting that phase-change material is utilized Make method, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 80-120 parts of phase transformation Material, 20-40 parts of styrene, 15-25 parts of methyl methacrylate, 3-7 parts of acrylic acid, 0.5-1.5 parts of silane are even Join 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, capsule-core of the phase-change material as phase-change microcapsule, styrene, methyl methacrylate Ester and acrylic acid form cyst wall by the way that polymerization reaction occurs as the reaction raw material of the cyst wall of phase-change microcapsule, eventually by Cyst wall coats capsule-core, forms microcapsules shape.Wherein as the crosslinking agent of polymerization reaction, azodiisobutyronitrile does silane coupling agent For the initiator of polymerization reaction, neopelex as emulsifier come using.It should be noted that phase transformation material therein For the phase transition temperature of material preferably between 30-35 DEG C, the quilt that the temperature-regulating fiber produced is processed into can be convenient people's sleep, 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 azobisisoheptonitrile or azo-bis-iso-dimethyl;Emulsifier can be with For 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 of aforementioned proportion and deionized water are stirred at 30-45 DEG C Water phase components are made in activation;
(4) emulsifying raw material: 30-45 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 5000-12000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5-20 hours at 80 DEG C, occurs poly- Reaction is closed, phase-change microcapsule lotion is made.Nitrogen protection can prevent influence of the oxygen to polymerization reaction, and oxygen is too active, It will affect efficiency of initiation, also will increase more side reaction in polymerization process.Certainly, protection gas can also use other indifferent gas Body, such as helium or argon gas
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80-100 DEG C, temperature-regulating fiber is made.Wherein, the fiber can be animal and plant fiber, such as cotton, fiber crops, silk, sheep Hair, cashmere etc.;It can be staple fibre, such as viscose rayon, copper ammonia fiber, acetate fiber;It can also be synthetic fibers, it is such as poly- In ester fiber, polyacrylonitrile fibre, Fypro etc. any one or any combination thereof fibrous material.
The present invention is described in further detail below by specific embodiment.Phase-change microcapsule of the invention and The characterization of the surface topography of temperature-regulating fiber and performance unless otherwise specified, uses following equipment:
Phase transformation dry using Jeol Ltd. JSM-5610LV type scanning electronic microscope observation, after metal spraying is micro- The surface topography of capsule.
Phase-change microcapsule is tested using Malvern Instr Ltd., Britain Mastersizer 2000E type laser particle analyzer Granularity.
Using platinum Ai Ermo Instrument Ltd., U.S. Pyris DimondC type differential scanning calorimeter (DSC), in nitrogen Under gas shielded, the DSC scanning curve of 10 DEG C/min temperature-rise period and -10 DEG C/min temperature-fall period is tested, it is micro- to obtain phase-change material The latent heat of phase change of capsule.
Using Wenzhou Darong Textile Instrument Co., Ltd. YG-606E type fabric heat-insulation ability meter in national standard side The heat preservation rate of temperature-regulating fiber is tested under method AATCC standard conditions.
The present invention does not address place and is suitable for the prior art.
Specific embodiments of the present invention are 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 production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 80 parts of capric acid, 20 The styrene, 15 parts of methyl methacrylate, 3 parts of acrylic acid, 0.5 part of silane coupling agent, 0.4 part of azo two of part are different Butyronitrile, 3 parts of neopelex and 500 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 30 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 30 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 81%.
The photo of the scanning electron microscope for the phase-change microcapsule that above-described embodiment obtains is as shown in Figure 1, obtained tune The photo of the scanning electron microscope of warm fiber is as shown in Figure 2.
Embodiment 2
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 120 parts of capric acid, 40 The styrene, 25 parts of methyl methacrylate, 7 parts of acrylic acid, 1.5 parts of silane coupling agent, 0.6 part of azo two of part are different Butyronitrile, 7 parts of neopelex and 700 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 30 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 30 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 84%.
Embodiment 3
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 30 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 30 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 85%.
Embodiment 4
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 110 parts of capric acid, 35 The styrene, 25 parts of methyl methacrylate, 6 parts of acrylic acid, 1.3 parts of silane coupling agent, 0.6 part of azo two of part are different Butyronitrile, 6 parts of neopelex and 650 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 30 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 30 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 82%.
Embodiment 5
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 86%.
Embodiment 6
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 45 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 45 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 45 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 5000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 84%.
Embodiment 7
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 7500r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 84%.
Embodiment 8
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 86%.
Embodiment 9
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 12000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heating 5 hours at 80 DEG C, and it is anti-that polymerization occurs It answers, phase-change microcapsule lotion is made.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 87%.
Embodiment 10
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) it monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heats 10 hours, polymerize at 80 DEG C Phase-change microcapsule lotion is made in reaction.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 84%.
Embodiment 11
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) it monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heats 15 hours, polymerize at 80 DEG C Phase-change microcapsule lotion is made in reaction.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 86%.
Embodiment 12
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) it monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heats 20 hours, polymerize at 80 DEG C Phase-change microcapsule lotion is made in reaction.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 80 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 87%.
Embodiment 13
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) it monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heats 10 hours, polymerize at 80 DEG C Phase-change microcapsule lotion is made in reaction.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 90 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 88%.
Embodiment 14
A kind of production method of temperature-regulating fiber, comprising the following steps:
Step 1: the preparation of phase-change microcapsule lotion
(1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 100 parts of capric acid, 30 Styrene, 20 parts of the methyl methacrylate, 5 parts of acrylic acid, 1 part of silane coupling agent, 0.5 part of two isobutyl of azo of part Nitrile, 5 parts of neopelex and 600 parts of water;
(2) prepared by oil phase component: the capric acid of aforementioned proportion, styrene, methyl methacrylate, acrylic acid, silane is even Connection agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 37 DEG C;
(3) water phase components prepare: by the dodecyl sodium sulfate of aforementioned proportion and deionized water at 37 DEG C stir-activating, Water phase components are made;
(4) emulsifying raw material: 37 DEG C at a temperature of, the oil phase component is added in water phase components, and with The revolving speed of 10000r/min is stirred emulsification, and homogeneous latex emulsion is made;
(5) it monomer polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, heats 10 hours, polymerize at 80 DEG C Phase-change microcapsule lotion is made in reaction.
Step 2: temperature-regulating fiber is prepared
Under conditions of 80 DEG C, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, then It is dried at 100 DEG C, temperature-regulating fiber is made.
Through detecting, 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, heat preservation Rate is 87%.
Test example: temperature-regulating fiber surface phase-change microcapsule adheres to uniformity testing
Test material: temperature-regulating fiber made from embodiment 10, embodiment 13 and embodiment 14, Publication No. Temperature-regulating fiber made from scheme used by the embodiment 3 recorded in the application for a patent for invention of CN104562258A, hereinafter referred to as Reference examples.
Test method: randomly select that embodiment 10, embodiment 13, temperature-regulating fiber is suitable prepared by embodiment 14 and reference examples Amount, is respectively cut the segment for 3mm, each embodiment randomly selects 10 sections of temperature-regulating fibers, using differential scanning calorimeter (DSC), DSC scanning curve under nitrogen protection, is drawn, the latent heat of phase change of every section of temperature-regulating fiber is obtained.And test result is remembered Record is in table 1.
By table 1 it is found that each portion of temperature-regulating fiber prepared by the embodiment of the present invention 10, embodiment 13 and embodiment 14 The extreme value and standard deviation for dividing the test result of potential heat value are all significantly lower than reference examples in the prior art, and the former test is equal Value is apparently higher than the latter, illustrates that the phase-change microcapsule particle on the obtained temperature-regulating fiber of technical solution of the present invention is distinguished very Uniformly, without significantly assembling or adhering to blind area, and potential heat value is apparently higher than similar product in the prior art.
1 temperature-regulating fiber surface phase-change microcapsule of table 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
Mean value 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 foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (9)

1. a kind of production method of temperature-regulating fiber, which comprises the following steps: step 1, phase-change microcapsule lotion Preparation: (1) raw material preparation: the phase-change microcapsule lotion includes the raw material of following parts by weight, 80-120 parts of capric acid, 20-40 parts of styrene, 15-25 parts of methyl methacrylate, 3-7 parts of acrylic acid, 0.5-1.5 parts of silane coupling agent, 0.4-0.6 parts of azodiisobutyronitrile, 3-7 parts of neopelex and 500-700 parts of deionized water, the capric acid Phase transition temperature be 30-35 DEG C;(2) prepared by oil phase component: by the capric acid of aforementioned proportion, styrene, methyl methacrylate, third Olefin(e) acid, silane coupling agent and azodiisobutyronitrile stir and evenly mix into oil phase component at 30~45 DEG C;(3) prepared by water phase components: By the neopelex of aforementioned proportion and deionized water at 30-45 DEG C stir-activating, be made water phase components;(4) former Material emulsification: 30-45 DEG C at a temperature of, the oil phase component is added in water phase components, and with 5000-12000r/min Revolving speed be stirred emulsification, be made homogeneous latex emulsion;(5) emulsion polymerization: under nitrogen protection by above-mentioned homogeneous latex emulsion, 80 It is heated 5-20 hours at DEG C, initiated polymerization, phase-change microcapsule lotion is made;Step 2 prepares temperature-regulating fiber: at 80 DEG C Under the conditions of, fiber is padded into 10-30min in the phase-change microcapsule lotion that step 1 obtains, is then dried at 80-100 DEG C, Temperature-regulating fiber is made.
2. the production method of temperature-regulating fiber according to claim 1, which is characterized in that the phase-change microcapsule lotion includes The raw material of following parts by weight, 100 parts of capric acid, 30 parts of styrene, 20 parts of methyl methacrylate, 5 parts of propylene Acid, 1 part of silane coupling agent, 0.5 part of azodiisobutyronitrile, 5 parts of neopelex and 600 parts of deionization Water.
3. the production method of temperature-regulating fiber according to claim 1, which is characterized in that water phase components, oil phase component preparation And the temperature of emulsifying raw material is 37 DEG C.
4. the production method of temperature-regulating fiber according to claim 1, which is characterized in that stirred during emulsifying raw material Revolving speed is 7500r/min.
5. the production method of temperature-regulating fiber according to claim 1, which is characterized in that heated in emulsion polymerization process Time is 10 hours.
6. the production method of temperature-regulating fiber according to claim 1, which is characterized in that the drying temperature in step 2 is 90 ℃。
7. a kind of temperature-regulating fiber, which is characterized in that be prepared using the described in any item production methods of claim 1~6.
8. temperature-regulating fiber according to claim 7, which is characterized in that the phase-change microcapsule adhered on the temperature-regulating fiber Mass fraction is 10%~30%.
9. a kind of thermostat quilt includes core and the back side, which is characterized in that core temperature adjustment as described in claim 7 or 8 is fine Dimension is made.
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CN102676123A (en) * 2012-04-10 2012-09-19 巢启 Microcapsule preparation method of phase change material
CN104117330B (en) * 2014-08-08 2015-12-09 广西启利新材料科技股份有限公司 The preparation method that a kind of low-temperature phase-change micro-capsule secondary is coated

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