CN106149095A - A kind of fabric lining containing hot energy storage material - Google Patents
A kind of fabric lining containing hot energy storage material Download PDFInfo
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- CN106149095A CN106149095A CN201610661681.5A CN201610661681A CN106149095A CN 106149095 A CN106149095 A CN 106149095A CN 201610661681 A CN201610661681 A CN 201610661681A CN 106149095 A CN106149095 A CN 106149095A
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- energy storage
- hot energy
- storage material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/12—Making microcapsules or microballoons by phase separation removing solvent from the wall-forming material solution
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F257/00—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
- C08F257/02—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00 on to polymers of styrene or alkyl-substituted styrenes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/02—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonates or saturated polyesters
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
Abstract
A kind of fabric lining containing hot energy storage material, it is characterised in that: containing hot energy storage material in fiber, this material is capsule form, and it contains the hot energy storage composition as core and shell component, comprises the steps: that (1) prepares hot energy storage material；(2) described hot energy storage material is mixed with spinning solution or spinning master batch；(3) high temperature extrusion stock solution or masterbatch mix；(4) fiber formed is collected.The hot energy storage material of the present invention can overcome high temperature during spinning, even if capsule is exposed to the spinning temperature more than 220 DEG C, core material is maintained to most or all of core material, we have found that when, after spinning technique, core material capsule can keep hydrophobic liquid or the wax of more than 99%.
Description
Technical field
The present invention relates to a kind of fabric lining containing hot energy storage material and preparation method thereof, belong to fibre manufacturing technology neck
Territory.
Background technology
(Phase Change Materials is called for short PCM to hot energy storage material.So-called hot energy storage refers to that material is in phase change
During absorb or release energy. this characteristic constitutes hot energy storage material and has wide variety of theoretical basis just.Heat storage
Can material from liquid to solid state transformation time, the change of physical state to be experienced.In both phase transition process, material will be from environment
Middle heat absorption, otherwise, to environment heat release.The energy that can store when physical state changes or discharge is referred to as the heat of transformation, occurs
The temperature range of phase transformation is the narrowest.When physical state changes, the temperature of material self almost remains unchanged before phase transformation completes.
When a large amount of heat of transformations are transferred in environment, create a wide temperature platform.The appearance of hot energy storage material, when embodying constant temperature
Between prolongation, and can store or discharge sensible heat with sensible heat and insulant when thermal cycle.Its principle is: hot energy storage material exists
Energy storage is got up by the transmitting procedure of heat, the energy transmission time can be extended just as thermal resistance, make thermograde
Reduce.By outward, using hot energy storage material also to have the advantage that one, phase transition process is usually isothermal or nearly quasi-isothermal process,
This characteristic is conducive to variations in temperature to maintain in less scope, makes human body feel comfortably cool；Its two, hot energy storage material has very
High latent heat of phase change, a small amount of material can store substantial amounts of heat.Microcapsule is the spherical vesicles with certain permeability, outward
Layer is semipermeable membrane, and inside is liquid core.Hot energy-storage fibre is to utilize to discharge or absorb latent heat, temperature guarantor in material phase transition process
Hold constant feature development a kind of heat-accumulation temperature-adjustment functional fibre out.The manufacture method of current hot energy-storage fibre mainly has: one,
Blending method, is divided into (1) hot energy storage material and polymer to be directly blended and carries out spinning, relatively simple but have that phase transformation heat content is low, phase
The problems such as the leakage that becomes different is low with fibre strength.It is easier to reality at present in the acrylon using wet spinning and cellulosic fibre
Existing.(2) microcapsule method (PCM).Microcapsule is to be closed by hot energy storage material parcel with macromolecule, prevents hot energy storage material from letting out
Leakage.Microcapsule containing hot energy storage material and polymer are carried out co-blended spinning and obtains phase change fiber, but there is bigger PCM meeting
It is filtered and fiber can not be entered and cause fiber enthalpy of phase change less；PCM and fibrous matrix poor compatibility cause fiber formidable opponent low
Problem.Two, composite spinning method.Core-sheath or island composite algorithm, enthalpy of phase change is relatively big, current fiber can accomplish 80J/g with
On, fibre diameter is 100 μm-3mm, can realize reusing after carrying out two ends or middle closing.Fill at clothing, work out
The aspect such as seat cushion, Car Cushion has preferable application prospect.And in recent years, microcapsule technology is widely used in microorganism, moves and plant
The immobilization aspect of thing cell, enzyme and other various bioactivators and chemicals.Conventional microcapsule is that alginic acid/poly-relies
Propylhomoserin microcapsule.Owing to technology of preparing is more complicated, the saccilar process time is longer, has certain to the biological activity of the material that is embedded
Impact, and the price comparison of polylysine is expensive, thus limit the use of this microcapsule.The stock preparing microcapsule leads to
Often there is the polyelectrolyte such as protein, lipid and sugar.Chitosan is the chitin of the de-Deacetylation degree of part, and the latter has excellent
Toughness and inertia, and hydrophilic, nontoxic, porous, uniformly, chitin content in nature is also the abundantest simultaneously.Existing
In technology, hot accumulation energy microcapsule technique is Hot spots for development in recent years and technological difficulties, as described in GB1507739A, base
In the capsule of melamine resin, it is impervious and durable, but they often have at high temperature impermeability
Relatively low shortcoming.And the material that WO9924525A describes, be not suitable for being exposed in high temperature.And it is specific currently without any one
Polymeric material is sufficiently strong, it is possible to tolerance high pressure, it is possible to the most still keep good hot energy storage effect.
Summary of the invention
For solving problem as above, the present invention adopts the following technical scheme that
A kind of fabric lining containing hot energy storage material, it is characterised in that: containing hot energy storage material in fiber, this material is capsule
Form, it contains the hot energy storage composition as core and shell component, comprises the steps:
(1) hot energy storage material is prepared；
(2) described hot energy storage material is mixed with spinning solution or spinning master batch；
(3) high temperature extrusion stock solution or masterbatch mix；
(4) fiber formed is collected.
Spinning solution or master batch are polyester, polypropylene, polylactic acid or polyurethane etc..
The preparation method of hot energy storage material, it is characterised in that comprise the steps:
(1) polystyrene solution is prepared by poly-for 3 15g (styrene) being dissolved in 80 100g styrene monomers, right
This mixture is stirred, until polymer is completely dissolved；
(2) by catalyst tetraisopropoxy titanium that mol ratio is the ethanedioic acid of 2:2:1.2, ethylene glycol, lactic acid and 0.2 0.9wt%
With phosphoric acid put into equipped with electronic reinforcement agitator, condensing reflux pipe two neck flasks in, under the protection of nitrogen, oil bath is heated to
After 200 300 DEG C, it is dehydrated 2 3h, then evacuation, controls pressure to vacuum less than 50Pa, carry out defat reaction, 2 5h
Rear stopped reaction, under the protection of nitrogen, the most i.e. obtains the high-molecular copolymer of white solid, is existed by products therefrom after cooling
It is vacuum dried at 30 50 DEG C.
(2) prepared by oil phase: weigh high-molecular copolymer prepared by 4 5mg steps (2), that prepared by 4 8g steps (1) is poly-
Styrene solution, 2 5g styrene, 2 3g methacrylic acids, 5 9g diethyleneglycol diacrylate are dissolved in l0mL dichloromethane
Alkane, until completely dissolved, is subsequently adding 150 200g hydrophobic liquid or waxes, is sufficiently stirred for and adds with ultrasonic cleaner instant
Solve, obtain oil phase.
(3) prepared by aqueous phase: measure 70 100mL deionized waters, adds 2 5wt% polyvinyl alcohol (PVA), is stirred by magnetic force
Mix device and stir 20 50min until being completely dissolved to obtain aqueous phase.
(4), after oil phase being joined aqueous phase, use cutter with rotating speed cutting 2 8min of 3000 9000rpm, prepare
Oil mixing with water emulsion, instills 100 300 μ L defoamer isoamyl alcohol.By emulsion on magnetic stirring apparatus constant temperature (25 35 DEG C) and
Low speed stirs 5 9h, treats that dichloromethane gradually volatilizees, and carrier material separates out, and finally solidify to form microcapsule suspensions.Gained is hanged
Supernatant liquid washing high speed centrifugation 2 times, removes supernatant, is dried 2 days in electrically heated drying cabinet (arranging temperature is 40 DEG C), both hot energy storage
Material.
Hydrophobic liquid or wax can be organic material.Such as, described hydrophobic liquid can be oil or molten wax.Excellent
Choosing, described hydrophobic liquid or wax are non-polymer material.It is further preferred that described hydrophobic liquid or wax are carbon
Hydrogen compound.Described oil or wax can comprise active material, such as, be dispersed or dissolved in UV absorbent therein, UV reflective agent
Or fire retardant.Therefore, described core material can be uniform, or it is alternatively possible to comprise and be scattered in throughout hydrophobicity liquid
The dispersion of the solid active material in the continuous core medium of body or wax.Described hydrophobic liquid or wax are that fusing point is-20 DEG C
The oil of 160 DEG C or wax.Can be C8-40 alkane, or can be cycloalkane.Suitable material includes all of alkane or cycloalkane
Isomer.Further, it is also possible to use the mixture of these alkane or cycloalkane.Can be (such as) selected from n-octadecane, positive ten
Four alkane, Pentadecane, n-heptadecane, n-octadecane, AI3-36122, n-docosane, n-tricosane, pentacosane, just
Any compound in hexacosane, hexamethylene, cyclooctane, cyclodecane and their isomer and/or their mixture.
The hot energy storage material of preparation discharges or absorbs energy at a temperature of 10 DEG C 150 DEG C, and half peak temperature is
At least 400 DEG C.
The mean diameter of microcapsule is 2 5um.
Compared with prior art, the application has the advantages that
1. high temperature when the hot energy storage material of the present invention can overcome spinning, even if capsule is exposed to the spinning temperature more than 220 DEG C
When spending, core material is maintained to most or all of core material, it has been found that when after spinning technique, core material glue
Capsule can keep hydrophobic liquid or the wax of more than 99%.
2. the shell of the hot energy storage material of the present invention has durability and impenetrability can make described capsule be incorporated into fiber
Or during fabric, there is no any significantly sacrificing.
Detailed description of the invention
Embodiment 1
(1) by poly-for 3g (styrene) (molecular weight is 1500) being dissolved in, to prepare polystyrene in 80g styrene monomer molten
Liquid, is stirred this mixture, until polymer is completely dissolved；
(2) by catalyst tetraisopropoxy titanium that mol ratio is the ethanedioic acid of 2:2:1.2, ethylene glycol, lactic acid and 0.9wt% and phosphorus
Acid put into equipped with electronic reinforcement agitator, condensing reflux pipe two neck flasks in, under the protection of nitrogen, oil bath is heated to 230 DEG C
After, it being dehydrated 2h, then evacuation, control pressure to vacuum less than 50Pa, carry out defat reaction, stopped reaction after 2h, at nitrogen
Under the protection of gas, after cooling, the most i.e. obtain the high-molecular copolymer of white solid, products therefrom is vacuum dried at 30 DEG C.
(2) prepared by oil phase: weigh high-molecular copolymer prepared by 4mg step (2), polystyrene prepared by 4g step (1)
Solution, 2g styrene, 2g methacrylic acid, 5g diethyleneglycol diacrylate be dissolved in l0mL dichloromethane, until completely dissolved,
It is subsequently adding 150g hydrophobic liquid or wax, is sufficiently stirred for and accelerates to dissolve with ultrasonic cleaner, obtaining oil phase.
(3) prepared by aqueous phase: measure 70mL deionized water, adds 2wt% polyvinyl alcohol (PVA), passes through magnetic stirrer
20min is until being completely dissolved to obtain aqueous phase.
(4), after oil phase being joined aqueous phase, use cutter with rotating speed cutting 2min of 3000rpm, prepare oil mixing with water
Emulsion, instills 100 μ L defoamer isoamyl alcohol.Emulsion constant temperature (25 DEG C) low speed on magnetic stirring apparatus are stirred 5h, treats dichloromethane
Alkane gradually volatilizees, and carrier material separates out, and finally solidify to form microcapsule suspensions.Gained suspension is washed high speed centrifugation 2 times,
Remove supernatant, in electrically heated drying cabinet (arranging temperature is 40 DEG C) be dried 2 days, both hot energy storage material.
Weigh 95kg polypropylene (pp) master batch, hot energy storage material 5kg, be placed in blender stirring 30 minutes, after stirring
Mixture dry four hours in the environment of 100 DEG C, be heated to 250 DEG C, then by double screw extruder extrude cellosilk, receive
Collection, then detection fibers silk intensity and fineness.
Embodiment 2
(1) prepare polystyrene solution by poly-for 8g (styrene) being dissolved in 90g styrene monomer, this mixture is entered
Row stirring, until polymer is completely dissolved；
(2) by catalyst tetraisopropoxy titanium that mol ratio is the ethanedioic acid of 2:2:1.2, ethylene glycol, lactic acid and 0.5wt% and phosphorus
Acid put into equipped with electronic reinforcement agitator, condensing reflux pipe two neck flasks in, under the protection of nitrogen, oil bath is heated to 230 DEG C
After, it being dehydrated 2h, then evacuation, control pressure to vacuum less than 50Pa, carry out defat reaction, stopped reaction after 3h, at nitrogen
Under the protection of gas, after cooling, the most i.e. obtain the high-molecular copolymer of white solid, products therefrom is vacuum dried at 40 DEG C.
(2) prepared by oil phase: weigh high-molecular copolymer prepared by 4mg step (2), polystyrene prepared by 8g step (1)
Solution, 4g styrene, 3g methacrylic acid, 6g diethyleneglycol diacrylate be dissolved in l0mL dichloromethane, until completely dissolved,
It is subsequently adding 160g hydrophobic liquid or wax, is sufficiently stirred for and accelerates to dissolve with ultrasonic cleaner, obtaining oil phase.
(3) prepared by aqueous phase: measure 80mL deionized water, adds 4wt% polyvinyl alcohol (PVA), passes through magnetic stirrer
35min is until being completely dissolved to obtain aqueous phase.
(4), after oil phase being joined aqueous phase, use cutter with rotating speed cutting 7min of 4000rpm, prepare oil mixing with water
Emulsion, instills 300 μ L defoamer isoamyl alcohol.Emulsion constant temperature (25 DEG C) low speed on magnetic stirring apparatus are stirred 6h, treats dichloromethane
Alkane gradually volatilizees, and carrier material separates out, and finally solidify to form microcapsule suspensions.Gained suspension is washed high speed centrifugation 2 times,
Remove supernatant, in electrically heated drying cabinet (arranging temperature is 40 DEG C) be dried 2 days, both hot energy storage material.
Weigh 100kg polylactic acid master batch, hot energy storage material 5kg, be placed in blender stirring 40 minutes, by mixing after stirring
Compound is dried four hours in the environment of 130 DEG C, is heated to 300 DEG C, is extruding cellosilk by double screw extruder, is collecting,
Then detection fibers silk intensity and fineness.
Comparative example 1
Hydrophobicity oil (comprising the polymer of addition) microcapsule
By mixing 4.94g styrene, 2.3g methacrylic acid, 4.76g poly-(styrene) solution (produced above) and
7.89g butanediol diacrylate prepares oil phase.Add the Alperox LP (deriving from ELF Atochem) of 1.4g, then add
Enter the hydrophobic liquid of 152g.
By mixing poly-(vinyl alcohol) (the deriving from the Gohsenol GH20R of Nippon Gohseii) of 5.4g, the water of 169g
And the Sodium AMPS (50% activity, derive from Lubrizol, France) of 0.64g prepares aqueous phase.
Aqueous phase and oil phase are warmed to 40 DEG C, and use Silverson L4R test chamber homogenizer that they are the most newborn
Change.After 10 minutes, obtain stable emulsion.
The emulsion of gained is poured in the reaction vessel that equipment is used for polyreaction, and be placed in the water-bath of 75 DEG C.Will
This temperature keeps 3 hours, and adds aqueous ammonium persulfate solution (0.6g, in 10g water).Polymeric material is heated to 80
DEG C, and stirring 2 hours at such a temperature, it is then cooled to room temperature, thus obtains end-product.This end-product is by the tool in water
Having the dispersion of the microcapsule of wax core and polymer shell, the mean diameter of wherein said microcapsule is 3 microns.
Fibre manufacture is with embodiment 1.
Comparative example 2
(1) prepared by carrier: by different for catalyst four that mol ratio is the succinic acid of 1:1:0.25, butanediol, lactic acid and 0.115wt%
Titanium propanolate and phosphoric acid put into equipped with electronic reinforcement agitator, condensing reflux pipe two neck flasks in, under the protection of nitrogen oil
After bath is heated to 240 DEG C, it is dehydrated 1h, then evacuation, controls pressure to vacuum less than 67Pa, carry out defat reaction, 3.5h
Rear stopped reaction, under the protection of nitrogen, the most i.e. obtains the high-molecular copolymer PBS-co-PLA of white solid, by institute after cooling
Obtain product to be vacuum dried at 60 DEG C.
(2) prepared by oil phase: accurately weighs 4mgPBS-co-PLA and is dissolved in l0mL dichloromethane, until completely dissolved, adds
The hydrophobic liquid of 1mg or wax, be sufficiently stirred for and accelerate to dissolve with ultrasonic cleaner, obtaining oil phase.
(3) prepared by aqueous phase: measure 98mL deionized water, adds 3wt%PVA-1788, by magnetic stirrer 40min
Until being completely dissolved to obtain aqueous phase.
(4) prepared by microcapsule: after oil phase is joined aqueous phase, uses cutter with rotating speed cutting 5min of 7000rpm, system
Obtain oil mixing with water emulsion, instill 150 μ L defoamer isoamyl alcohol.Emulsion constant temperature (28 DEG C) low speed on magnetic stirring apparatus are stirred
8h, treats that dichloromethane gradually volatilizees, and carrier material separates out, and finally solidify to form microcapsule suspensions.Gained suspension is washed
High speed centrifugation 3 times, removes supernatant, is dried 1 day, had both obtained microcapsule finished product in electrically heated drying cabinet (arranging temperature is 45 DEG C).
Fibre manufacture is with embodiment 2.
Analyze
Particle diameter
Use the Sympatec Analyser (deriving from Sympatec GmbH) being provided with Quixcel disperse system and R4 lens
Carry out granularmetric analysis.
Thermogravimetric analysis (TGA)
Using temperature range is that the Perkin Elmer TGA of 110 DEG C to 500 DEG C is to carry out thermogravimetric analysis.
Table 1
1Half-peak: it is at half peak heights of attenuation curve.
2Mass loss at 300 DEG C: it is that the material deriving from sample between initial conditions, 110 DEG C and 300 DEG C damages
The amount (representing with the form of percentage rate) lost.
3Gross weight (monomer adds hydrophobic polymer) based on polymer shell.
The highest by half peak value half-peak value in contrast table, then microcapsule is to rupturing (this is due to intrinsic pressure formation)
Resistance the highest, i.e. shell wall is the firmest.
Compared with the present invention, other preparation method of comparative example can cause the character of microcapsule (to be damaged by effective quality
Lose and measure) deterioration.
Claims (8)
1. the fabric lining containing hot energy storage material, it is characterised in that: containing hot energy storage material in fiber, this material is glue
Scrotiform formula, it contains the hot energy storage composition as core and shell component.
2. the preparation method of fiber as claimed in claim 1, it is characterised in that comprise the steps:
(1) hot energy storage material is prepared；
(2) described hot energy storage material is mixed with spinning solution or spinning master batch；
(3) high temperature extrusion stock solution or masterbatch mix；
(4) fiber formed is collected.
3. preparation method as claimed in claim 2, it is characterised in that the preparation method of hot energy storage material comprises the steps:
(1) polystyrene solution is prepared by poly-for 3 15g (styrene) being dissolved in 80 100g styrene monomers, right
This mixture is stirred, until polymer is completely dissolved；
(2) by catalyst tetraisopropoxy titanium that mol ratio is the ethanedioic acid of 2:2:1.2, ethylene glycol, lactic acid and 0.2 0.9wt%
With phosphoric acid put into equipped with electronic reinforcement agitator, condensing reflux pipe two neck flasks in, under the protection of nitrogen, oil bath is heated to
After 200 300 DEG C, it is dehydrated 2 3h, then evacuation, controls pressure to vacuum less than 50Pa, carry out defat reaction, 2 5h
Rear stopped reaction, under the protection of nitrogen, the most i.e. obtains the high-molecular copolymer of white solid, is existed by products therefrom after cooling
It is vacuum dried at 30 50 DEG C；
(2) prepared by oil phase: weigh high-molecular copolymer prepared by 4 5mg steps (2), polyphenyl second prepared by 4 8g steps (1)
Alkene solution, 2 5g styrene, 2 3g methacrylic acids, 5 9g diethyleneglycol diacrylate are dissolved in l0mL dichloromethane, treat
After being completely dissolved, it is subsequently adding 150 200g hydrophobic liquid or waxes, is sufficiently stirred for and accelerates to dissolve with ultrasonic cleaner,
Oil phase；
(3) prepared by aqueous phase: measure 70 100mL deionized waters, adds 2 5wt% polyvinyl alcohol (PVA), passes through magnetic stirring apparatus
Stir 20 50min until being completely dissolved to obtain aqueous phase；
(4), after oil phase being joined aqueous phase, use cutter with rotating speed cutting 2 8min of 3000 9000rpm, prepare profit
Mixed emulsion, instills 100 300 μ L defoamer isoamyl alcohol, emulsion constant temperature on magnetic stirring apparatus is stirred 5 9h, treats dichloromethane
Alkane gradually volatilizees, and carrier material separates out, and finally solidify to form microcapsule suspensions, gained suspension is washed high speed centrifugation, goes
Supernatant, at electrically heated drying cabinet, temperature be 40 DEG C in be dried, both hot energy storage material.
4. the preparation method described in claim 3, it is characterised in that described hydrophobic liquid or wax are Hydrocarbon.
5. the preparation method described in claim 3, it is characterised in that: described hydrophobic liquid or wax be fusing point be-20 DEG C 160
DEG C oil or wax.
6. preparation method as claimed in claim 3, it is characterised in that the hot energy storage material of preparation is at 10 DEG C 150 DEG C
At a temperature of discharge or absorb energy, and half peak temperature is at least 400 DEG C.
7. preparation method as claimed in claim 2, it is characterised in that: described high temperature is at least 220 DEG C.
8. preparation method as claimed in claim 3, it is characterised in that: spinning solution or master batch are polyester, polypropylene, polylactic acid
Or polyurethane.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111270327A (en) * | 2020-03-31 | 2020-06-12 | 孙阁 | Anti-mosquito and anti-mite functional fiber and preparation method thereof |
| CN114561743A (en) * | 2021-12-13 | 2022-05-31 | 杭州诺邦无纺股份有限公司 | Preparation method of phase-change non-woven material |
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