CN106758266A - Microcapsules and its preparation method and application and temperature-regulation fabric for preparing temperature-regulation fabric - Google Patents
Microcapsules and its preparation method and application and temperature-regulation fabric for preparing temperature-regulation fabric Download PDFInfo
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- CN106758266A CN106758266A CN201611109749.5A CN201611109749A CN106758266A CN 106758266 A CN106758266 A CN 106758266A CN 201611109749 A CN201611109749 A CN 201611109749A CN 106758266 A CN106758266 A CN 106758266A
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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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- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
-
- 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
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
-
- 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
- D06M13/11—Compounds containing epoxy groups or precursors 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
- 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
- D06M13/12—Aldehydes; Ketones
- D06M13/123—Polyaldehydes; Polyketones
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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
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
-
- 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
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/13—Alginic acid or derivatives thereof
-
- 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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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a kind of preparation method for preparing the microcapsules of temperature-regulation fabric, will include that the mixed liquor of sodium alginate and calcium carbonate mixes with paraffin and water oil compound emulsifying agent first, carry out emulsion reaction, obtain emulsion oil-in-water；Then the emulsion oil-in-water for obtaining mixes with petroleum ether and acid flux material, carries out curing reaction, obtains primary microcapsules；The primary microcapsules that will then obtain carry out condensation reaction with shitosan acid solution, obtain textile surface coating microcapsules.The result of embodiment shows that the temperature-regulation fabric of the microcapsules that the surface coating present invention is prepared, by after the washing of 1~5 time, mass loss rate is below 5%, illustrates that phase-change material is good with substrate fabric firmness.
Description
Technical field
The invention belongs to weaving face fabric production technical field, and in particular to a kind of microcapsules for preparing temperature-regulation fabric
And its preparation method and application and temperature-regulation fabric.
Background technology
With the increasingly raising of people's living standard, requirement more and more higher of the people to weaving face fabric function.Temperature adjustment is weaved
Product are that one kind can release energy when temperature is low, and heat is absorbed after temperature is uprised, and reduce the novel intelligent textile of temperature；
Temperature-regulation fabric has the effect that Double-direction Temperature is adjusted, being capable of automatic absorption, storage, distribution and releasing energy, raising wearer
Comfort level.
The preparation principle of temperature-regulation fabric is the surface that phase-changing and temperature-regulating material is added to textile, and prepared by direct fabrics
Phase-changing and temperature-regulating fiber is weaved or blending again.The preparation method of temperature-regulation fabric mainly has finishing method, doughnut method, spins
Silk method and foam method.Although the temperature-regulation fabric that prior art can be prepared, due to the limitation of technique and formula,
During subsequent use, firmness is poor between phase-change material and textile for the temperature-regulation fabric for preparing, phase-change material meeting
As the increase of washing times comes off from textile surface, temperature adjusting performance is lost.Such as Chinese patent CN200810061268.8
A kind of preparation method of intelligent thermoregulation type functional yarn is disclosed, it is specific to disclose phase-change microcapsule dispersion liquid and thickener, glue
The functional finishing agent that mixture is configured to, rolls through two leachings two or slashing technique is arranged onto yarn, then by follow-up weaving technology system
Obtain temperature-regulation fabric；But the invention is arranged from finished microcapsule emulsion to yarn, and microcapsules and yarn had not been considered
The binding ability of line, causes temperature-regulation fabric microcapsules during follow-up use to come off, and loses temperature adjusting performance.For another example, China
Patent CN201410407505.X discloses a kind of intelligent temperature-regulation fabric and preparation method thereof, using binders for coatings to phase transformation
After microcapsules carry out parcel mixing, it is coated on weaving face fabric surface and is prepared from, but the program prepares temperature-regulation fabric
Still suffer from the problem of coating and substrate fastness difference.
The content of the invention
It is an object of the invention to provide a kind of microcapsules for preparing temperature-regulation fabric and its preparation method and application
And temperature-regulation fabric, it is intended to a kind of phase-change material and the good temperature-regulation fabric of base material firmness can be provided.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides a kind of preparation method for preparing the microcapsules of temperature-regulation fabric, comprise the following steps：
(1) will include that the mixed liquor of sodium alginate and calcium carbonate mixes with paraffin and water oil compound emulsifying agent, emulsified
Reaction, obtains emulsion oil-in-water；
(2) emulsion oil-in-water that the step (1) is obtained is mixed with petroleum ether and acid flux material, solidify instead
Should, obtain primary microcapsules；
(3) primary microcapsules that the step (2) obtains carry out condensation reaction with shitosan acid solution, obtain temperature adjustment spinning
Fabric microcapsules.
Preferably, the mass ratio of sodium alginate, calcium carbonate and water is (1~3) in the mixed liquor of the step (1):(0.5
~1.5)：(80~100).
Preferably, step (1) the reclaimed water oil compound emulsifying agent includes aqueous emulsifier phase and oil phase emulsifier, the oil phase
The mass ratio of emulsifying agent and the aqueous emulsifier phase is (6~8)：(3~4).
Preferably, shitosan and the mass ratio of the sodium alginate are (2 in shitosan acid solution in the step (3)
~4)：(1~3), the mass fraction of shitosan acid solution is 0.2~1.0% in the step (3).
It is described the invention provides the microcapsules that preparation method described in above-mentioned technical proposal is obtained, including capsule-core and cyst wall
Capsule-core includes paraffin, and the cyst wall includes sodium alginate and shitosan.
Preferably, the mass ratio of the paraffin, sodium alginate and shitosan is (1~3)：(1~3)：(2~4).
The invention provides the microcapsules described in above-mentioned technical proposal as coating adhesive in temperature-regulation fabric is prepared should
With, including：Coating sizing material containing the microcapsules is coated in the web surface containing amino and/or hydroxyl, cross-linking reaction
Obtain temperature-regulation fabric.
Preferably, the coating sizing material includes microcapsules and bleeding agent, adhesive and thickener；
The fabric carries out precrosslink reaction in being soaked in crosslinking agent before coating, and the crosslinking agent shrinks for ethylene glycol two
Glycerin ether or glutaraldehyde；
Cross-linking reaction after the applying coating sizing material is carried out under the conditions of baking.
Preferably, described baking baked with secondary including baking first, and the temperature for baking first is 100~120 DEG C,
The time for baking first is 10~20min；The secondary temperature for baking be 150~160 DEG C, it is described it is secondary bake when
Between be 2~4min.
The invention provides the temperature-regulation fabric that above-mentioned application is prepared, including the fabric containing amino and/or hydroxyl
With the coating glue-line for being coated in the web surface, the coating glue-line is connected with fabric by cross-linking agents.
The invention provides a kind of preparation method for preparing the microcapsules of temperature-regulation fabric, first will be including alginic acid
The mixed liquor of sodium and calcium carbonate mixes with paraffin and water oil compound emulsifying agent, carries out emulsion reaction, obtains emulsion oil-in-water；So
The emulsion oil-in-water for obtaining afterwards mixes with petroleum ether and acid flux material, carries out curing reaction, obtains primary microcapsules；Then will
The primary microcapsules for obtaining carry out condensation reaction with shitosan acid solution, obtain temperature-regulation fabric microcapsules.In the present invention
In, including sodium alginate mixed liquor and paraffin pass through water oil compound emulsifying agent effect, while realizing to oil-soluble paraffin
With the emulsion process of water miscible sodium alginate, promote both split-phases, emulsion oil-in-water is obtained, with reference to follow-up petroleum ether
With the mixing of acid flux material, oil phase is well dispersed in petroleum ether, and water is mutually well dispersed in calcium carbonate aqueous solution, calcium from
Son promotes the solidification of sodium alginate in acid condition, realizes parcel of the sodium alginate to paraffin wax；It is wrapped in paraffin surface
Sodium alginate a large amount of negatively charged carboxyls are provided, while being produced in chitosan molecule chain in being dissolved in acid solution a large amount of
Positively charged primary amino radical, and then there is condensation reaction in shitosan and sodium alginate, realize that shell gathers by the attraction of positive and negative charge
Sugar for microcapsules subsequently provide basis with the crosslinking of textile, and then is improved as phase-change material to the second layer parcel of paraffin
Capsule-core and fabric firmness, obtain using paraffin as capsule-core, using sodium alginate and shitosan as the microcapsules of cyst wall.It is real
The result for applying example shows, the temperature-regulation fabric of the microcapsules that the surface coating present invention is prepared, by after the washing of 1~5 time,
Mass loss rate is below 5%, illustrates that phase-change material is good with substrate fabric firmness.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the grain size distribution of the microcapsules that the embodiment of the present invention 3 is prepared；
Fig. 2 prepares microcapsules and textile mechanism of crosslinking schematic diagram for the embodiment of the present invention 3；
Fig. 3 prepares microcapsules and textile cross-linking reaction infrared spectrogram for the embodiment of the present invention 8.
Specific embodiment
The invention provides a kind of preparation method for preparing the microcapsules of temperature-regulation fabric, comprise the following steps：
(1) will include that the mixed liquor of sodium alginate and calcium carbonate mixes with paraffin and water oil compound emulsifying agent, emulsified
Reaction, obtains emulsion oil-in-water；
(2) emulsion oil-in-water that the step (1) is obtained is mixed with petroleum ether and acid flux material, solidify instead
Should, obtain primary microcapsules；
(3) primary microcapsules that the step (2) obtains carry out condensation reaction with shitosan acid solution, obtain temperature adjustment spinning
Fabric microcapsules.
The present invention will include that the mixed liquor of sodium alginate and calcium carbonate mixes with paraffin and water oil compound emulsifying agent.In this hair
In bright, the mass ratio of sodium alginate, calcium carbonate and water is preferably (1~3) in the mixed liquor：(0.5~1.5)：(80~
100), more preferably (1.5~2)：(1.0~1.5)：(85~90).The present invention is environmentally friendly, nontoxic using sodium alginate, full
The requirement of the textile of foot and direct body contact.
In the present invention, the mixed liquor of the sodium alginate and calcium carbonate is preferably prepared under the conditions of 45~60 DEG C,
More preferably 50~55 DEG C；It is able to ensure that sodium alginate and calcium carbonate fully dissolve at said temperatures.
After the mixing, sodium alginate, calcium carbonate, paraffin and water oil compound emulsifying agent carry out emulsion reaction, obtain water bag
Water emulsion.In the present invention, the consumption of the paraffin and water oil compound emulsifying agent is preferably with sodium alginate in the mixed liquor
Quality on the basis of count, the paraffin, water oil compound emulsifying agent and the mass ratio of sodium alginate are preferably (1~3)：(6~14)：
(1~3), more preferably (1.5~2)：(8~10)：(1.5~2).In the present invention, the water oil compound emulsifying agent is excellent
Choosing includes aqueous emulsifier phase and oil phase emulsifier, and the oil phase emulsifier is preferably Tween-80, and the aqueous emulsifier phase is preferably
Arlacel-80；The mass ratio of the oil phase emulsifier and aqueous emulsifier phase is preferably (6~8)：(3~4), more preferably
(6.5~7)：(3.5~3.8).The no particular/special requirement in source to the Tween-80 and Arlacel-80 of the invention, using this area
Known to technical staff.In the present invention, the paraffin is preferably paraffin wax；In the present invention, the section stone
Wax purity is high, it is to avoid excessively polymictic introducing.
In the present invention, the time of the emulsion reaction be preferably 30~50min, more preferably 35~45min.
In the present invention, oil phase emulsifier can realize the emulsification to oil-soluble paraffin, and aqueous emulsifier phase can be realized to water miscible
The emulsification of sodium alginate, realizes the separation of water phase and an oil phase, obtains emulsion oil-in-water.
After the emulsion reaction, the present invention mixes the emulsion oil-in-water for obtaining with petroleum ether and acid flux material,
Curing reaction is carried out, primary microcapsules are obtained.In the present invention, the consumption of the petroleum ether and acid flux material is preferably with described mixed
Counted on the basis of the quality for closing the sodium alginate in liquid, the mass ratio of the petroleum ether, acid flux material and sodium alginate is preferably (80
~100) (0.25~1.25)：(1~3), more preferably (85~95) (0.5~1.2)：(1.5~2.5), more preferably
90：1.0：2.In the present invention, the acid flux material be preferably one kind in formic acid, acetic acid, propionic acid, benzoic acid and ethanedioic acid or
It is various.
In the present invention, the curing reaction is preferably carried out under agitation, and time of the stirring is preferably 10~
30min, more preferably 15~25min, more preferably 20min；In the present invention, the rotating speed of the stirring is preferably 1000
~2000rpm, more preferably 1500~1800rpm.The present invention does not have special wanting to the source of the petroleum ether and acetic acid
Ask, using petroleum ether well-known to those skilled in the art and acetic acid.
The present invention, during the curing reaction, oil phase is dispersed in petroleum ether in the emulsion oil-in-water, water
Mutually it is dispersed in calcium carbonate soln, in acid condition, the calcium ion in calcium carbonate promotes sodium alginate to solidify, and then obtains
Sodium alginate wraps up the primary microcapsules of paraffin.
After completing the curing reaction, the present invention preferably curing reaction product mixes with calcium chloride water, carries out
Curing reaction, obtains primary microcapsules again.In the present invention, in the calcium chloride water quality of calcium chloride can realize
Hydroxyl on microcapsules ground floor shell sodium alginate can form ionic bond and be defined；In the present invention, the calcium chloride is water-soluble
The consumption of liquid preferably to be counted on the basis of the quality of sodium alginate in the mixed liquor, the quality of shown calcium chloride water with it is described
The mass ratio of sodium alginate is preferably (80~100)：(1~3), more preferably (85~90)：(1.5~2).In the present invention
In, the concentration of the calcium chloride water is preferably 0.05~0.2mol/L, more preferably 0.1~0.15mol/L.
In the present invention, the curing reaction again is preferably carried out under agitation, and the time of the stirring is preferably
10~30min, more preferably 12~25min, more preferably 20min；In the present invention, the rotating speed of the stirring is preferably
2000~2500rpm, more preferably 2200~2300rpm.In the present invention, the addition of the calcium chloride solution is further
The solidification of sodium alginate, raising is promoted to be wrapped in the stability of the sodium alginate on paraffin wax surface.
The primary microcapsules for obtaining and shitosan acid solution cleaned after condensation reaction, dried by the present invention,
Obtain temperature-regulation fabric microcapsules.
In the present invention, the consumption of the shitosan acid solution is preferably in terms of the quality of shitosan, with the alginic acid
The mass ratio of sodium is preferably (2~4)：(1~3), more preferably (2.5~3.5)：(1.5~2.5), more preferably 3:2.
In the present invention, the mass concentration of the shitosan acid solution be preferably 0.2~1.0%, more preferably 0.5~
0.8%；In the present invention, the solvent of the shitosan acid solution is preferably acetum；In the present invention, the acetic acid is molten
The concentration of liquid is preferably 0.2%~1.0%, more preferably 0.5%~0.8%；In the present invention, the shitosan is acid
The pH value of solution is preferably 3~4, more preferably 3.5~3.8.Under the regulation of acetum of the present invention, mixing water
Calcium ion in solution solidifies to sodium alginate.
Preferably be soaked in the primary microcapsules in the shitosan acid solution by the present invention, carries out condensation reaction；
In the present invention, the soak time is preferably 0.5~2.5h, more preferably 1~2h.The present invention is in the immersion process
In, the sodium alginate for being wrapped in paraffin surface provides a large amount of negatively charged carboxyls, while shitosan is dissolved in acid solution
A large amount of positively charged primary amino radicals, and then shitosan and sodium alginate are produced to be contracted by the attraction of positive and negative charge on strand
Reaction is closed, second layer parcel of the shitosan to paraffin is realized, for microcapsules subsequently provide basis, Jin Erti with the crosslinking of textile
Capsule-core and the firmness of fabric as phase-change material high.
After completing the condensation reaction, the product that the preferred cleaning of the present invention and the drying condensation reaction are obtained is adjusted
Temperature microcapsules used for textiles.In the present invention, the mode of the cleaning preferably uses dimethylbenzene, absolute ethyl alcohol and distillation successively
Water is rinsed；The present invention does not have particular/special requirement to the number of times of the cleaning, in an embodiment of the present invention, the dimethylbenzene, anhydrous
The washing time of ethanol and distilled water is specially 3 times, 3 times and 4 times respectively.The present invention is to the concrete mode of the flushing without spy
It is different to require, using cleaning way well-known to those skilled in the art.
After completing the flushing, the present invention is dried after the flushing product preferably is carried out into suction filtration.The present invention is to institute
Stating suction filtration does not have particular/special requirement, using suction filtration well-known to those skilled in the art, is produced with that can realize that separation of solid and liquid obtains solid-state
Thing is defined.Solid product obtained by preferred pair of the present invention is dried, and the dry temperature is preferably 50~60 DEG C, enters one
Step is preferably 52~55 DEG C.The present invention does not have particular/special requirement to the dry time, can remove residual water in solid product
Divide and residual solvent is defined.
In the present invention, the cleaning, suction filtration and drying can realize the auxiliary material removal to being introduced in preparation process,
In the present invention, the auxiliary material is calcium carbonate, compound emulsifying agent, petroleum ether, acetic acid, calcium chloride and acid flux material.
Present invention also offers the microcapsules that above-mentioned technical proposal is prepared, including capsule-core and cyst wall, the capsule-core bag
Paraffin is included, the cyst wall includes sodium alginate and shitosan.In the present invention, the sodium alginate is preferably as the first cyst wall bag
The paraffin surface is overlying on, the shitosan is coated on the first cyst wall table preferably as the second cyst wall by condensation reaction
Face.In the present invention, the mass ratio of the paraffin, sodium alginate and shitosan is (1~3)：(1~3)：(2~4), further
Preferably (1.5~2.5)：(1.5~2.5)：(2.5~3.5), more preferably 2:2:3.In the present invention, as micro- glue
The presence of the second cyst wall shitosan of capsule, to provide connection site as the phase-change material of capsule-core and the connection of textile fabric.
The invention provides the microcapsules described in above-mentioned technical proposal as coating adhesive in temperature-regulation fabric is prepared should
With, including：Coating sizing material containing the microcapsules is coated in the web surface containing amino and hydroxyl, cross-linking reaction is obtained
Temperature-regulation fabric.
In the present invention, the coating sizing material preferably includes microcapsules, bleeding agent, adhesive and thickener.In the present invention
In, the mass ratio of the microcapsules, bleeding agent, adhesive and thickener is preferably (10~50)：(5~25)：(30~50)：
(10~30), more preferably (15~20)：(15~20)：(35~45)：(15~20), more preferably 18：18：36：18.
The present invention commercially available is oozed to the no particular/special requirement in source of the bleeding agent using well-known to those skilled in the art
Saturating agent.In the present invention, the bleeding agent is preferably the HFS-2 type bleeding agents of the preferred company's production of Dandong fixed star chemical industry.
The present invention adds bleeding agent in the coating sizing material, contributes to coating sizing material to be realized to face liber after web surface coating
Infiltration, and bleeding agent dispersion and emulsion effect is good, it is possible to increase the capillary effect and whiteness of fabric, while improving fabric feeling.
In the present invention, the thickener is preferably propylene carboxylic acids polymer；Source of the present invention to the thickener
There is no particular/special requirement, using commercially available propylene carboxylic acids polymer well-known to those skilled in the art；In the present invention, institute
State the FD-200A type thickeners of the preferred company's production of thickener specially Dandong fixed star chemical industry.
In the present invention, described adhesive is preferably polyacrylate polymers or modifier；The present invention is to described poly-
The no particular/special requirement in source of acrylic polymer or modifier, using commercial binder well known to those skilled in the art
；In the present invention, described adhesive is specially the FS-465 type environment-friendly adhesives of the preferred company's production of Dandong fixed star chemical industry.
In the present invention, before the coating, the fabric carries out precrosslink reaction, the friendship in being preferably soaked in crosslinking agent
Connection agent is ethylene glycol diglycidylether or glutaraldehyde.
The fabric that the present invention is provided contains amino and/or hydroxyl；In the present invention, the amino is preferably Amino End Group, institute
State hydroxyl preferably Amino End Group；In the present invention, the material of the fabric be preferably one kind in silk, cotton-polyester fabric and nylon or
It is various；The present invention does not have particular/special requirement to the form of fabric of the fabric, is knitted using fabric well-known to those skilled in the art
Thing；In an embodiment of the present invention, the fabric is specially using 28tex × 28tex cotton plains cloth.
Be soaked in the fabric in crosslinking agent and carry out precrosslink reaction by the present invention.In the present invention, the crosslinking agent
Consumption on the basis of the quality of capsule-core in the microcapsules preferably to count, and the quality of the crosslinking agent is excellent with the mass ratio of the capsule-core
Elect as (6~10)：(1~3), more preferably (7~8)：(1.5~2).In the present invention, precrosslink reaction when
Between be preferably 10~30min, more preferably more preferably 15~25min, 20min.In precrosslink reaction of the present invention,
One end group of the crosslinking agent reacts with the amino or hydroxyl contained by textile, realizes between the crosslinking agent and fabric
Connection；The other end of the crosslinking agent still retains the functional group not reacted for the connection with microcapsules, crosslinking agent reality
Bridging microcapsules and fabric are showed.Phase-change microcapsule of the present invention crosslinks the mechanism of reaction as shown in Fig. 2 crosslinking with textile
Agent serves bridging and contains the fabric of hydroxyl and/or carboxyl in the effect of microcapsules.
In the present invention, the crosslinking agent is ethylene glycol diglycidylether or glutaraldehyde.Shunk when using ethylene glycol two
When glycerin ether is as crosslinking agent, the ether of ethylene glycol diglycidylether one end reacts with the amino of fabric, hydroxyl, another
End retains the ether not reacted can react with the amino in the follow-up shitosan for adding and hydroxyl, and ethylene glycol two shrinks
Glycerin ether played bridging microcapsules with and textile effect；When using glutaraldehyde as crosslinking agent, glutaraldehyde one end
Aldehyde radical reacts with the amino and/or hydroxyl of fabric, and the other end retains the aldehyde radical not reacted and gathers with the follow-up shell for adding
Amino and hydroxyl in sugar react, glutaraldehyde played bridging microcapsules with and textile effect.
In the present invention, the cross-linking reaction for being carried out after the applying coating sizing material is carried out preferably under the conditions of baking.At this
In invention, it is described bake to preferably include to bake first baked with secondary；In the present invention, the roasting first and after baking
Interval time preferably 0~5min, more preferably 0.5~2min.Liter of the present invention to roasting and the after baking first
Warm speed does not have particular/special requirement, can obtain target sintering temperature.In the present invention, the temperature for baking first is preferred
It is 100~120 DEG C, more preferably 105~115 DEG C, more preferably 110 DEG C；The time for baking first is preferably 10
~20min, more preferably 12~18min, more preferably 15min；In the present invention, the secondary temperature for baking is preferred
It is 150~160 DEG C, more preferably 152~158 DEG C, more preferably 155 DEG C；The secondary time for baking is preferably 2~
4min, more preferably 2.5~3.5min, more preferably 3min.
In the present invention, specifically, the preparation method of the temperature-regulation fabric preferably includes following steps：
Microcapsules described in above-mentioned technical proposal are mixed with bleeding agent, adhesive and thickener, coating sizing material is obtained；
Fabric containing amino and/or hydroxyl is provided；
The fabric is soaked in carries out precrosslink reaction in crosslinking agent, the crosslinking agent is ethylene glycol diglycidylether
Or glutaraldehyde；
Cross-linking reaction is carried out after the reacted web surface of the precrosslink coats the coating sizing material, temperature adjustment spinning is obtained
Fabric；The cross-linking reaction is carried out under the conditions of baking.
In the present invention, the coating sizing material is preferably prepared according to the method for comprising the following steps：By micro- glue
Capsule adds adhesive to be stirred first after mixing with the bleeding agent, adds thickener and continues to stir, and obtains coating sizing material.
In the present invention, described adhesive is preferably added under agitation, and the rotating speed that described adhesive is stirred when adding is preferably 500
~1200rpm；In the present invention, the rotating speed for stirring first is preferably 500~1000rpm, more preferably 700~
800rpm；In the present invention, the time stirred first be defined so that the intermixture that viscosity is 5000~6000CPS can be obtained；
In the present invention, the rotating speed for continuing to stir is preferably 500~1000rpm, more preferably 550~650rpm；It is described
The time for continuing to stir is preferably 30~60min, more preferably 40~45min.
After completing the precrosslink reaction of the fabric, the present invention is described in the reacted web surface coating of the precrosslink
Cross-linking reaction is carried out after coating sizing material, temperature-regulation fabric is obtained.The present invention does not have special restriction for the mode of the coating,
Using the technical scheme of coating well known to those skilled in the art.Directly coated present invention preferably employs dry method.The present invention
For carrying out the used equipment of the coating there is no special restriction, using well known to those skilled in the art for coating
Equipment.The coating is carried out present invention preferably employs scraper type coating machine.In the present invention, the coating amount of the coating adhesive
It is preferred that making dry weightening of the fabric after baking be 10~15g/m2, more preferably 12~14g/m2, most preferably 13g/m2.At this
In invention, the coating sizing material forms phase-change material coating in web surface, fabric is had good temperature adjusting performance.
After completing the coating, the present invention preferably carries out stewing process, and the time of the standing is preferably 5~10min, enters
One step is preferably 6~8min.In the present invention, the stewing process contributes to the firm of coating.
Fabric after the standing is preferably carried out cross-linking reaction by the present invention, obtains temperature-regulation fabric；The cross-linking reaction
Carried out under roasting condition.In the present invention, it is described bake process with baked described in above-mentioned technical proposal it is consistent, herein not
Repeat again.
The invention provides the temperature-regulation fabric that above-mentioned technical proposal is prepared, including containing amino and/or hydroxyl
Fabric and the coating glue-line for being coated in the web surface, the coating glue-line are connected with fabric by cross-linking agents.This hair
In the temperature-regulation fabric of bright offer, the crosslinking agent is firmly attached to web surface by crosslinking reaction with fabric, while
Crosslinking agent is connected with the second cyst wall shitosan in the microcapsules in coating adhesive component by cross-linking reaction, realizes microcapsules and fabric
Firm connection；The coating adhesive has the characteristic of phase-changing and temperature-regulating, fabric is had the function of temperature adjustment, heat accumulation thermal.
Below in conjunction with the embodiment in the present invention, the technical scheme in the present invention is clearly and completely described.It is aobvious
So, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the reality in the present invention
Example is applied, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made all belongs to
In the scope of protection of the invention.
In following examples and comparative example, used bleeding agent is the JFS-2 of Dandong fixed star Chemical Co., Ltd. production
Type high-efficient penetrant；Thickener used is the FS-200A type thickeners of Dandong fixed star Chemical Co., Ltd. production；Adhesive therefor
It is the FS-465 type environment-friendly adhesives of Dandong fixed star Chemical Co., Ltd. production.
Embodiment 1
The preparation of microcapsules：In parts by mass, by 80 parts of water of 1.0 parts of sodium alginates and 0.5 part of calcium carbonate at 45 DEG C
Dissolving, (water oil compound emulsifying agent is that mass ratio is 6 to add 1.0 parts of paraffin waxs and 6 parts of water oil compound emulsifying agents:4 tween-
80 and Arlacel-80) after carry out emulsification 30min, obtain emulsion oil-in-water；By emulsion oil-in-water be dispersed in 80 parts of petroleum ethers with
In 0.25 part of acetic acid mixture, 10min is stirred with the rotating speed of 2000rpm, the calcium chloride for adding 80 parts of 0.05mol/L is water-soluble
Liquid, equally stirs 10min with the rotating speed of 2000rpm, obtains the primary microcapsules that sodium alginate wraps up paraffin wax；To prepare
Primary microcapsules be placed in the chitosan-acetic acid solution that mass concentration is 0.2%, wherein the mass parts of shitosan be 2 parts immersion
0.5h, suction filtration after using dimethylbenzene cleaning 3 times, the mode that washes of absolute alcohol cleans 4 times 3 times with distilled water to be cleaned successively
Separation of solid and liquid is realized, last 50 DEG C dry removal residual moisture and residual solvent, obtain microcapsules.
The pretreatment of textile：By 28tex × 28tex cottons plain cloth in 6 parts of ethylene glycol diglycidyls of mass parts
10min is soaked in ether.
The preparation of temperature-regulation fabric：5 parts of bleeding agents are mixed with 10 parts of microcapsules, and adds 30 parts to glue with 500rpm stirrings
It is 6000CPS to sticky state that mixture is stirred to viscosity with the rotating speed of 800rpm, 10 parts of thickeners is eventually adding, with 500rpm's
Rotating speed continues to stir 30min, obtains the coating adhesive containing microcapsules.The coating adhesive scraper that will be prepared is scratched in treated spinning
Fabric surface, blade coating stable 5min after terminating, 100 DEG C of preliminary drying 20min, 150 DEG C of trainings are dried 2min, do weightening 15g/m2, adjusted
Warm textile.
Embodiment 2
The preparation of microcapsules：In parts by mass, by 85 parts of water of 1.5 parts of sodium alginates and 0.75 part of calcium carbonate at 45 DEG C
Dissolving, (water oil compound emulsifying agent is that mass ratio is 6 to add 1.5 parts of paraffin waxs and 8 parts of water oil compound emulsifying agents:4 tween-
80 and Arlacel-80) after carry out emulsification 35min, obtain emulsion oil-in-water；By emulsion oil-in-water be dispersed in 85 parts of petroleum ethers with
In 0.5 part of acetic acid mixture, 10min is stirred with the rotating speed of 2000rpm, adds 85 parts of calcium chloride waters of 0.05mol/L,
The same rotating speed with 2000rpm stirs 10min, obtains the primary microcapsules that sodium alginate wraps up paraffin wax；By what is prepared
Primary microcapsules are placed in the chitosan-acetic acid solution that mass concentration is 0.4%, soak 1h, the wherein relative mass of shitosan part
It is 2.5 parts, is cleaned 3 times using dimethylbenzene successively, after the mode that washes of absolute alcohol cleans 4 times 3 times with distilled water is cleaned
Suction filtration realizes separation of solid and liquid, and last 50 DEG C dry removal residual moisture and residual solvent, obtain microcapsules.
The pretreatment of textile：By 28tex × 28tex cottons plain cloth in 7 parts of ethylene glycol diglycidyls of mass parts
15min is soaked in ether.
The preparation of temperature-regulation fabric：10 parts of bleeding agents are mixed with 20 parts of microcapsules, and 35 parts are added with 500rpm stirrings
It is 5000CPS to sticky state that adhesive is stirred to viscosity with the rotating speed of 700rpm, 15 parts of thickeners is eventually adding, with 500rpm
Rotating speed continue stir 30min, obtain the coating adhesive containing microcapsules.The coating adhesive scraper that will be prepared is scratched in treated
Textile surface, blade coating stable 5min after terminating, 100 DEG C of preliminary drying 20min, 150 DEG C of trainings are dried 2min, do weightening 15g/m2, obtain
Temperature-regulation fabric.
Embodiment 3
The preparation of microcapsules：In parts by mass, by 90 parts of water of 2.0 parts of sodium alginates and 1.0 parts of calcium carbonate at 45 DEG C
Dissolving, (water oil compound emulsifying agent is that mass ratio is 6 to add 2.0 parts of paraffin waxs and 10 parts of water oil compound emulsifying agents:4 tween-
80 and Arlacel-80) after carry out emulsification 40min, obtain emulsion oil-in-water；By emulsion oil-in-water be dispersed in 90 parts of petroleum ethers with
In 0.75 part of acetic acid mixture, 15min is stirred with the rotating speed of 2000rpm, the calcium chloride for adding 90 parts of 0.05mol/L is water-soluble
Liquid, equally stirs 15min with the rotating speed of 2000rpm, obtains the primary microcapsules that sodium alginate wraps up paraffin wax；To prepare
Primary microcapsules be placed in the chitosan-acetic acid solution that mass concentration is 0.6%, soak 1.5h, wherein, 2 parts of quality of shitosan
Part, cleaned 3 times using dimethylbenzene successively after immersion, after the mode that washes of absolute alcohol cleans 4 times 3 times with distilled water is cleaned
Suction filtration realizes separation of solid and liquid, and last 50 DEG C dry removal residual moisture and residual solvent, obtain microcapsules.
The pretreatment of textile：By 28tex × 28tex cottons plain cloth in 8 parts of ethylene glycol diglycidyls of mass parts
20min is soaked in ether.
The preparation of temperature-regulation fabric：15 parts of bleeding agents are mixed with 30 parts of microcapsules, and 40 parts are added with 500rpm stirrings
Adhesive is stirred to viscosity as 6000CPS with the rotating speed of 500rpm, is eventually adding 20 parts of thickeners, is continued with the rotating speed of 500rpm
Stirring 30min, obtains the coating adhesive containing microcapsules.The coating adhesive scraper that will be prepared is scratched in treated textile table
Face, blade coating stable 5min after terminating, 100 DEG C of preliminary drying 20min, 150 DEG C of trainings are dried 2min, do weightening 15g/m2, obtain temperature adjustment weaving
Product.
Embodiment 4
The preparation of microcapsules：In parts by mass, by 95 parts of water of 2.5 parts of sodium alginates and 1.25 parts of calcium carbonate at 55 DEG C
Dissolving, (water oil compound emulsifying agent is that mass ratio is 6 to add 2.5 parts of paraffin waxs and 12 parts of water oil compound emulsifying agents:4 tween-
80 and Arlacel-80) after carry out emulsification 45min, obtain emulsion oil-in-water；By emulsion oil-in-water be dispersed in 95 parts of petroleum ethers with
In 1.0 parts of acetic acid mixtures, 20min is stirred with the rotating speed of 2000rpm, adds 95 parts of calcium chloride waters of 0.05mol/L,
The same rotating speed with 2000rpm stirs 20min, obtains the primary microcapsules that sodium alginate wraps up paraffin wax；By what is prepared
Primary microcapsules are placed in the chitosan-acetic acid solution that mass concentration is 0.8%, soak 2.0h, and shell gathers in chitosan-acetic acid solution
The mass fraction of sugar is 3.5 parts, successively using dimethylbenzene cleaning 3 times, washes of absolute alcohol 3 times and distilled water cleaning 4 after immersion
Suction filtration realizes separation of solid and liquid after secondary mode is cleaned, and last 50 DEG C dry removal residual moisture and residual solvent, obtain micro-
Capsule.
The pretreatment of textile：By 28tex × 28tex cottons plain cloth in 9 parts of ethylene glycol diglycidyls of mass parts
25min is soaked in ether.
The preparation of temperature-regulation fabric：20 parts of bleeding agents are mixed with 40 parts of microcapsules, and 45 parts are added with 500rpm stirrings
Adhesive is stirred to viscosity as 6000CPS with the rotating speed of 800rpm, is eventually adding 25 parts of thickeners, is continued with the rotating speed of 500rpm
Stirring 30min, obtains the coating adhesive containing microcapsules.The coating adhesive scraper that will be prepared is scratched in treated textile table
Face, blade coating stable 5min after terminating, 100 DEG C of preliminary drying 20min, 150 DEG C of trainings are dried 2min, do weightening 15g/m2, obtain temperature adjustment weaving
Product.
Embodiment 5
The preparation of microcapsules：In parts by mass, by 100 parts of water of 3.0 parts of sodium alginates and 1.5 parts of calcium carbonate at 60 DEG C
Dissolving, (water oil compound emulsifying agent is that mass ratio is 6 to add 3.0 parts of paraffin waxs and 14 parts of water oil compound emulsifying agents:4 tween-
80 and Arlacel-80) after carry out emulsification 50min, obtain emulsion oil-in-water；Emulsion oil-in-water is dispersed in 100 parts of petroleum ethers
In 1.25 parts of acetic acid mixtures, 30min is stirred with the rotating speed of 2000rpm, add 100 parts of calcium chloride water of 0.05mol/L
Solution, equally stirs 10min with the rotating speed of 2000rpm, obtains the primary microcapsules that sodium alginate wraps up paraffin wax；To prepare
Good primary microcapsules are placed in the chitosan-acetic acid solution that mass concentration is 1.0%, soak 0.5h, and wherein shitosan acetic acid is molten
Shitosan is 4 parts of mass parts in liquid, is then cleaned 3 times using dimethylbenzene successively, and washes of absolute alcohol 3 times and distilled water clean 4
Suction filtration realizes separation of solid and liquid after secondary mode is cleaned, and last 50 DEG C dry removal residual moisture and residual solvent, obtain micro-
Capsule.
The pretreatment of textile：By 28tex × 28tex cottons plain cloth in 6 parts of ethylene glycol diglycidyls of mass parts
10min is soaked in ether.
The preparation of temperature-regulation fabric：25 parts of bleeding agents are mixed with 50 parts of microcapsules, and 50 parts are added with 500rpm stirrings
Adhesive is stirred to viscosity as 5000CPS with the rotating speed of 800rpm, is eventually adding 30 parts of thickeners, is continued with the rotating speed of 500rpm
Stirring 30min, obtains the coating adhesive containing microcapsules.The coating adhesive scraper that will be prepared is scratched in treated textile table
Face, blade coating stable 5min after terminating, 100 DEG C of preliminary drying 20min, 150 DEG C of trainings are dried 2min, do weightening 15g/m2, obtain temperature adjustment weaving
Product.
Embodiment 6
The preparation of microcapsules：In parts by mass, by 80 parts of water of 1.0 parts of sodium alginates and 0.5 part of calcium carbonate at 45 DEG C
Dissolving, (water oil compound emulsifying agent is that mass ratio is 6 to add 1.0 parts of paraffin waxs and 6 parts of water oil compound emulsifying agents:4 tween-
80 and Arlacel-80) after carry out emulsification 30min, obtain emulsion oil-in-water；By emulsion oil-in-water be dispersed in 80 parts of petroleum ethers with
In 0.25 part of acetic acid mixture, 10min is stirred with the rotating speed of 2000rpm, obtain the primary micro- of sodium alginate parcel paraffin wax
Capsule；The primary microcapsules that will be prepared are placed in the chitosan-acetic acid solution that mass concentration is 0.2%, soak 0.5h, wherein
The quality of shitosan is 2.0 parts in chitosan-acetic acid solution, is cleaned 3 times using dimethylbenzene successively after immersion, washes of absolute alcohol 3
Secondary and distilled water cleans suction filtration after the mode of 4 times is cleaned and realizes separation of solid and liquid, last 50 DEG C dry removal residual moistures and
Residual solvent, obtains microcapsules.
The pretreatment of textile：By 28tex × 28tex cottons plain cloth in 6 parts of ethylene glycol diglycidyls of mass parts
10min is soaked in ether.
The preparation of temperature-regulation fabric：5 parts of bleeding agents are mixed with 10 parts of microcapsules, and adds 30 parts to glue with 500rpm stirrings
It is 6000CPS to sticky state that mixture is stirred to viscosity with the rotating speed of 800rpm, 10 parts of thickeners is eventually adding, with 500rpm's
Rotating speed continues to stir 30min, obtains the coating adhesive containing microcapsules.The coating adhesive scraper that will be prepared is scratched in treated spinning
Fabric surface, blade coating stable 5min after terminating, 100 DEG C of preliminary drying 20min, 150 DEG C of trainings are dried 2min, do weightening 15g/m2, adjusted
Warm textile.
Embodiment 7
The preparation of microcapsules：In parts by mass, by 85 parts of water of 1.5 parts of sodium alginates and 0.75 part of calcium carbonate at 45 DEG C
Dissolving, (water oil compound emulsifying agent is that mass ratio is 6 to add 1.5 parts of paraffin waxs and 8 parts of water oil compound emulsifying agents:4 tween-
80 and Arlacel-80) after carry out emulsification 35min, obtain emulsion oil-in-water；By emulsion oil-in-water be dispersed in 85 parts of petroleum ethers with
In 0.5 part of acetic acid mixture, 10min is stirred with the rotating speed of 2000rpm, obtain primary micro- glue that sodium alginate wraps up paraffin wax
Capsule；The primary microcapsules that will be prepared are placed in the chitosan-acetic acid solution that mass concentration is 0.4%, soak 1h, shitosan vinegar
The quality of shitosan is 2.5 parts in acid solution, successively using dimethylbenzene cleaning 3 times, washes of absolute alcohol 3 times and distillation after immersion
Suction filtration realizes separation of solid and liquid after the mode that water cleaning is 4 times is cleaned, and last 50 DEG C dry removal residual moisture and residual solvents,
Obtain microcapsules.
The pretreatment of textile：By 28tex × 28tex cottons plain cloth in 7 parts of ethylene glycol diglycidyls of mass parts
15min is soaked in ether.
The preparation of temperature-regulation fabric：10 parts of bleeding agents are mixed with 20 parts of microcapsules, and 35 parts are added with 500rpm stirrings
It is 5000CPS to sticky state that adhesive is stirred to viscosity with the rotating speed of 700rpm, 15 parts of thickeners is eventually adding, with 500rpm
Rotating speed continue stir 30min, obtain the coating adhesive containing microcapsules.The coating adhesive scraper that will be prepared is scratched in treated
Textile surface, blade coating stable 5min after terminating, 100 DEG C of preliminary drying 20min, 150 DEG C of trainings are dried 2min, do weightening 15g/m2, obtain
Temperature-regulation fabric.
Embodiment 8
The preparation of microcapsules：In parts by mass, by 80 parts of water of 1.0 parts of sodium alginates and 0.5 part of calcium carbonate at 45 DEG C
Dissolving, (water oil compound emulsifying agent is that mass ratio is 6 to add 1.0 parts of paraffin waxs and 6 parts of water oil compound emulsifying agents:4 tween-
80 and Arlacel-80) after carry out emulsification 30min, obtain emulsion oil-in-water；By emulsion oil-in-water be dispersed in 80 parts of petroleum ethers with
In 0.25 part of acetic acid mixture, 10min is stirred with the rotating speed of 2000rpm, the calcium chloride for adding 80 parts of 0.05mol/L is water-soluble
Liquid, equally stirs 10min with the rotating speed of 2000rpm, obtains the primary microcapsules that sodium alginate wraps up paraffin wax；To prepare
Primary microcapsules be placed in the chitosan-acetic acid solution that mass concentration is 0.2% soak, wherein shitosan be 2.0 mass parts,
Cleaned 3 times using dimethylbenzene successively after immersion 0.5h, the mode that washes of absolute alcohol cleans 4 times 3 times with distilled water is cleaned
Suction filtration realizes separation of solid and liquid afterwards, and last 50 DEG C dry removal residual moisture and residual solvent, obtain microcapsules.
The pretreatment of textile：28tex × 28tex cottons plain cloth is soaked in 6 parts of glutaraldehydes of mass parts
10min。
The preparation of temperature-regulation fabric：5 parts of bleeding agents are mixed with 10 parts of microcapsules, and adds 30 parts to glue with 500rpm stirrings
It is 6000CPS to sticky state that mixture is stirred to viscosity with the rotating speed of 800rpm, 10 parts of thickeners is eventually adding, with 500rpm's
Rotating speed continues to stir 30min, obtains the coating adhesive containing microcapsules.The coating adhesive scraper that will be prepared is scratched in treated spinning
Fabric surface, blade coating stable 5min after terminating, 100 DEG C of preliminary drying 20min, 150 DEG C of trainings are dried 2min, do weightening 15g/m2, adjusted
Warm textile.
Comparative example 1
5 parts of bleeding agents are mixed with 30 parts of adhesives, and is stirred to viscosity as 6000CPS with 500rpm, add 10 parts of increasings
Thick dose, 30min is stirred with 500rpm rotating speeds.The coating adhesive scraper that will be prepared is scratched in textile surface, and blade coating is steady after terminating
Determine 5min, 100 DEG C of preliminary drying 20min, 160 DEG C of trainings are dried 2min, do weightening 15g/m2。
Comparative example 2
10 parts of bleeding agents are mixed with 35 parts of adhesives, and is stirred to viscosity as 5000CPS with 500rpm, add 15 parts of increasings
Thick dose, stir 30min.The coating adhesive scraper that will be prepared is scratched in textile surface, blade coating stable 5min, 100 DEG C after terminating
2min is dried in preliminary drying 20min, 160 DEG C of trainings, does weightening 15g/m2。
Comparative example 3
15 parts of bleeding agents are mixed with 40 parts of adhesives, and is stirred to viscosity as 6000CPS with 500rpm, add 20 parts of increasings
Thick dose, stir 30min.The coating adhesive scraper that will be prepared is scratched in textile surface, blade coating stable 5min, 110 DEG C after terminating
2min is dried in preliminary drying 15min, 160 DEG C of trainings, does weightening 15g/m2。
Comparative example 4
20 parts of bleeding agents are mixed with 45 parts of adhesives, and is stirred to viscosity as 6000CPS with 500rpm, add 25 parts of increasings
Thick dose, stir 30min.The coating adhesive scraper that will be prepared is scratched in textile surface, blade coating stable 5min, 110 DEG C after terminating
2min is dried in preliminary drying 15min, 160 DEG C of trainings, does weightening 15g/m2。
Comparative example 5
25 parts of bleeding agents are mixed with 50 parts of adhesives, and it is 6000CPS to sticky state to be stirred to viscosity with 500rpm,
30 parts of thickeners are added, 30min is stirred.The coating adhesive scraper that will be prepared is scratched in textile surface, and blade coating is stable after terminating
5min, 120 DEG C of preliminary drying 10min, 160 DEG C of trainings are dried 2min, do weightening 15g/m2。
The microcapsules that embodiment 3 is prepared are tested using Malvern laser particle analyzer, as a result as shown in Figure 1.
As shown in Figure 1, the microcapsules that prepared by the present invention are nanoscale, between most microcapsule particle diameters are distributed in 20~40nm, explanation
The phase-change microcapsule particle diameter is smaller, it is easier to contacted with textile, provides strong for microcapsules and textile crosslink reaction
Ensure.
Preparing temperature-regulation fabric to the embodiment of the present invention 8 carries out infrared analysis, as a result as shown in figure 3, wherein 1 is phase
Become microcapsules infared spectrum, 2 is shitosan infared spectrum, and 3 is the infrared curve that embodiment 3 prepares temperature-regulation fabric, is led to
Cross contrast, it is seen that No. 3 have new functional group to produce.As shown in Figure 3 in 1553cm-1Place has strong absworption peak, this explanation shell
Glycan amino crosslinks generation schiff bases with crosslinking agent；In 3085cm-1There is an absworption peak in place, and this is the hydroxyl of textile
Reacted generation unsaturation C=C double bonds with crosslinking agent, it is seen that consistent, the crosslinking agent that is connected mechanism Fig. 2 with textile with microcapsules
Serve bridging and contain the fabric of hydroxyl and/or carboxyl in the effect of microcapsules.
Performance test is carried out to fabric prepared by embodiment 1~5 and comparative example 1~5, and coating is set not contain microcapsules
28tex × 28tex cotton plain cloth fabrics as control, wherein, according to GB/T 8629-2001 Textile Tests family
Washing and drying program are washed to the textile for preparing, and the mass loss rate after fabric washing is as shown in table 1, wherein
It is calculated on the basis of quality when accordingly the mass loss rate after number of times is not to wash.
Mass loss rate after fabric washing prepared by 1 embodiment of table 1~5
As can be seen from Table 1, the temperature-regulation fabric that the embodiment of the present invention 1~5 is prepared after washing, mass loss rate
5% is below, and as the increase of washing times, mass loss rate are still maintained at less than 5%, illustrates that the present invention is prepared into
The temperature-regulation fabric excellent washfastness for arriving, while also illustrating the painting containing microcapsules in the temperature-regulation fabric that the present invention is prepared
Layer glue is strong with fabric excellent bonding performance, fastness.
Textile phase transition temperature, heat content performance parameter, are surveyed using Mettler-Toledo DSC-822/400 types heat analysis
Examination instrument is tested, 0 DEG C~80 DEG C of Range of measuring temp, 5 DEG C/min of heating rate, and atmosphere is nitrogen；It is cold using contacting
Warm sense test instrument maximum heat value of the test containing microcapsule phase-change textile, and the heat conduction system of textile is calculated according to formula I
Number, characterizes the heat conductivility of textile.Test result is as shown in table 2 and table 3.
In formula I：K is thermal conductivity factor (W/m DEG C)；
D is textile samples thickness (m)；
A is the area (㎡ of hot plate)；
Δ T is the temperature difference (DEG C) between upper and lower hot plate；
W is heat flow (w).
The performance test results of the temperature-regulation fabric that the embodiment 1~8 of table 2 is prepared：
The comparative example 1~5 of table 3 prepares the performance test results of textile
From table 2 and table 3, the textile that the microcapsules prepared through the present invention were arranged, with unfinished weaving
Condition ratio, its thermal conductivity factor becomes big, and with the increase of microcapsules consumption, thermal conductivity factor k increases therewith, and this can be explained,
The microcapsules that the present invention is prepared can increase the thermal conductivity factor of textile.
The textile after washing of embodiment 1~8 its thermal conductivity factor is declined slightly, but its heat conductivility is still better than without micro-
The textile that capsule is arranged, it is seen that microcapsules crosslink reaction in the presence of crosslinking agent with textile, are firmly attached to
Fiber surface, it is difficult for drop-off in water-washing process, therefore thermal conductivity factor decline is little.Equally, spinning of the embodiment 1~8 containing microcapsules
There is phase in version test temperature is interval in fabric, and with certain latent heat of phase change, phase transition temperature near 50 DEG C, this with cut
The phase transition temperature (51.21 DEG C) of piece paraffin is close, and comparative example 1~5 is not detected without the textile that phase-change microcapsule is arranged
Phase transition temperature, microcapsules prepared by this explanation present invention assign the performance of textile phase-changing and temperature-regulating, with certain heat accumulation thermal
Ability.
The data of Integrated comparative table 1, table 2 and table 3, it is known that, calcium chloride solution is subsequently added, washing fastness has obtained more entering
The raising of one step, the further solidification that promotion sodium alginate is added again of calcium chloride solution, further makes carboxylic on sodium alginate
Base forms ionic bond, strengthens the intensity of microcapsules ground floor shell, it is ensured that be fully cured, it is to avoid strength of microcapsules is not enough and rupture
The not enough problem of later stage latent heat then.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method for preparing the microcapsules of temperature-regulation fabric, comprises the following steps：
(1) will include that the mixed liquor of sodium alginate and calcium carbonate mixes with paraffin and water oil compound emulsifying agent, carry out emulsion reaction,
Obtain emulsion oil-in-water；
(2) emulsion oil-in-water that the step (1) is obtained is mixed with petroleum ether and acid flux material, carries out curing reaction, obtained
To primary microcapsules；
(3) primary microcapsules that the step (2) obtains carry out condensation reaction with shitosan acid solution, obtain temperature-regulation fabric
Use microcapsules.
2. preparation method according to claim 1, it is characterised in that sodium alginate, carbon in the mixed liquor of the step (1)
The mass ratio of sour calcium and water is (1~3):(0.5~1.5)：(80~100).
3. preparation method according to claim 1, it is characterised in that step (1) the reclaimed water oil compound emulsifying agent includes
The mass ratio of aqueous emulsifier phase and oil phase emulsifier, the oil phase emulsifier and the aqueous emulsifier phase is (6~8)：(3~4).
4. preparation method according to claim 1, it is characterised in that shell in shitosan acid solution in the step (3)
Glycan is (2~4) with the mass ratio of the sodium alginate：(1~3), the quality of shitosan acid solution point in the step (3)
Number is 0.2~1.0%.
5. the microcapsules that the preparation method described in any one of Claims 1 to 4 is prepared, including capsule-core and cyst wall, its feature
It is：The capsule-core includes paraffin, and the cyst wall includes sodium alginate and shitosan.
6. microcapsules according to claim 5, it is characterised in that the mass ratio of the paraffin, sodium alginate and shitosan
It is (1~3)：(1~3)：(2~4).
7. application of the microcapsules described in claim 5 or 6 as coating adhesive in temperature-regulation fabric is prepared, including：To contain
The coating sizing material of the microcapsules is coated in the web surface containing amino and/or hydroxyl, and cross-linking reaction obtains temperature-regulation fabric.
8. application according to claim 7, it is characterised in that the coating sizing material includes microcapsules with bleeding agent, bonding
Agent and thickener；
The fabric carries out precrosslink reaction in being soaked in crosslinking agent before coating, and the crosslinking agent is ethylene glycol diglycidyl
Ether or glutaraldehyde；
Cross-linking reaction after the applying coating sizing material is carried out under the conditions of baking.
9. application according to claim 8, it is characterised in that described baking baked with secondary including baking first, described
The temperature for baking first is 100~120 DEG C, and the time for baking first is 10~20min；The secondary temperature that bakes is
150~160 DEG C, the secondary time for baking is 2~4min.
10. the temperature-regulation fabric prepared in being applied described in any one of claim 7~9, including contain amino and/or hydroxyl
Fabric and be coated in the coating glue-line of the web surface, the coating glue-line is connected with fabric by cross-linking agents.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611109749.5A CN106758266A (en) | 2016-12-06 | 2016-12-06 | Microcapsules and its preparation method and application and temperature-regulation fabric for preparing temperature-regulation fabric |
Applications Claiming Priority (1)
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Cited By (11)
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| CN107868986A (en) * | 2017-06-22 | 2018-04-03 | 浙江宝娜斯袜业有限公司 | Possesses the textile of temperature adjustment function |
| CN108951159A (en) * | 2018-07-11 | 2018-12-07 | 黄勇 | A kind of textile softener |
| CN109137115A (en) * | 2018-08-29 | 2019-01-04 | 中科纺织研究院（青岛）有限公司 | A kind of intelligent temperature adjusting fiber cellulose fiber and preparation process |
| CN109701461A (en) * | 2018-10-25 | 2019-05-03 | 西南交通大学 | A kind of preparation and its application of the calcium carbonate based on PEG/Dex aqueous two-phase/calcium alginate compounded micro-capsule |
| CN109722885A (en) * | 2018-12-26 | 2019-05-07 | 江南大学 | A kind of preparation method of type of heat heat accumulation thermal comfortable textile product |
| CN109881478A (en) * | 2019-03-08 | 2019-06-14 | 中服帽饰创意研发南通有限公司 | A kind of antimicrobial health care function scrambled eggs fabric and preparation method thereof |
| CN111560687A (en) * | 2020-05-25 | 2020-08-21 | 潘燚 | Thermal-inductance warm-keeping functional fabric and preparation method thereof |
| CN112411198A (en) * | 2020-10-22 | 2021-02-26 | 苏州逸纪杰电子科技有限公司 | Flame-retardant temperature-regulating environment-friendly non-woven fabric and preparation method thereof |
| CN112746376A (en) * | 2020-12-23 | 2021-05-04 | 杭州宏达装饰布织造有限公司 | Preparation method of knitted fabric with adjustable temperature |
| CN116751354A (en) * | 2023-07-11 | 2023-09-15 | 苏州健能新材料科技有限公司 | Lignin bio-based flame-retardant polyurethane foam joint mixture and preparation method thereof |
| CN116807938A (en) * | 2023-07-06 | 2023-09-29 | 希肤科技（上海）有限公司 | Composite mask cloth with color-changing function and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107868986A (en) * | 2017-06-22 | 2018-04-03 | 浙江宝娜斯袜业有限公司 | Possesses the textile of temperature adjustment function |
| CN108951159A (en) * | 2018-07-11 | 2018-12-07 | 黄勇 | A kind of textile softener |
| CN109137115A (en) * | 2018-08-29 | 2019-01-04 | 中科纺织研究院（青岛）有限公司 | A kind of intelligent temperature adjusting fiber cellulose fiber and preparation process |
| CN109701461B (en) * | 2018-10-25 | 2021-06-08 | 西南交通大学 | Preparation and application of PEG/Dex double aqueous phase-based calcium carbonate/calcium alginate composite microcapsule |
| CN109701461A (en) * | 2018-10-25 | 2019-05-03 | 西南交通大学 | A kind of preparation and its application of the calcium carbonate based on PEG/Dex aqueous two-phase/calcium alginate compounded micro-capsule |
| CN109722885A (en) * | 2018-12-26 | 2019-05-07 | 江南大学 | A kind of preparation method of type of heat heat accumulation thermal comfortable textile product |
| CN109881478A (en) * | 2019-03-08 | 2019-06-14 | 中服帽饰创意研发南通有限公司 | A kind of antimicrobial health care function scrambled eggs fabric and preparation method thereof |
| CN111560687A (en) * | 2020-05-25 | 2020-08-21 | 潘燚 | Thermal-inductance warm-keeping functional fabric and preparation method thereof |
| CN112411198A (en) * | 2020-10-22 | 2021-02-26 | 苏州逸纪杰电子科技有限公司 | Flame-retardant temperature-regulating environment-friendly non-woven fabric and preparation method thereof |
| CN112746376A (en) * | 2020-12-23 | 2021-05-04 | 杭州宏达装饰布织造有限公司 | Preparation method of knitted fabric with adjustable temperature |
| CN116807938A (en) * | 2023-07-06 | 2023-09-29 | 希肤科技（上海）有限公司 | Composite mask cloth with color-changing function and preparation method thereof |
| CN116807938B (en) * | 2023-07-06 | 2024-04-16 | 希肤科技（上海）有限公司 | Composite mask cloth with color-changing function and preparation method thereof |
| CN116751354A (en) * | 2023-07-11 | 2023-09-15 | 苏州健能新材料科技有限公司 | Lignin bio-based flame-retardant polyurethane foam joint mixture and preparation method thereof |
| CN116751354B (en) * | 2023-07-11 | 2024-02-09 | 苏州健能新材料科技有限公司 | Lignin bio-based flame-retardant polyurethane foam joint mixture and preparation method thereof |
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