CN113832735B - Polylactic acid porous nanofiber-nanometer phase change capsule composite material and preparation method and application thereof - Google Patents
Polylactic acid porous nanofiber-nanometer phase change capsule composite material and preparation method and application thereof Download PDFInfo
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- CN113832735B CN113832735B CN202010582995.2A CN202010582995A CN113832735B CN 113832735 B CN113832735 B CN 113832735B CN 202010582995 A CN202010582995 A CN 202010582995A CN 113832735 B CN113832735 B CN 113832735B
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- 239000002775 capsule Substances 0.000 title claims abstract description 70
- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 68
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 68
- 230000008859 change Effects 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002121 nanofiber Substances 0.000 claims abstract description 35
- 239000011159 matrix material Substances 0.000 claims abstract description 28
- 239000011148 porous material Substances 0.000 claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 16
- 239000000839 emulsion Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 3
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 46
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 27
- 235000021314 Palmitic acid Nutrition 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 17
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 16
- 238000009987 spinning Methods 0.000 claims description 16
- 241000208125 Nicotiana Species 0.000 claims description 11
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010041 electrostatic spinning Methods 0.000 claims description 10
- 239000012046 mixed solvent Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000003995 emulsifying agent Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000002114 nanocomposite Substances 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 2
- 238000003980 solgel method Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 11
- 239000000835 fiber Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 5
- 238000011068 loading method Methods 0.000 abstract description 3
- 239000003431 cross linking reagent Substances 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 12
- 239000012782 phase change material Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 8
- 239000002088 nanocapsule Substances 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 235000019504 cigarettes Nutrition 0.000 description 6
- 239000003546 flue gas Substances 0.000 description 6
- 239000011162 core material Substances 0.000 description 5
- 239000003094 microcapsule Substances 0.000 description 5
- 230000000391 smoking effect Effects 0.000 description 5
- 239000000779 smoke Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/061—Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/17—Filters specially adapted for simulated smoking devices
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
- D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/14—Thermal energy storage
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The invention discloses a polylactic acid porous nanofiber-nanometer phase change capsule composite material, a preparation method and application thereof, wherein the composite material comprises a polylactic acid porous nanofiber matrix and nanometer phase change capsules attached in nanometer pores of the polylactic acid porous nanofiber matrix, and the particle size of the nanometer phase change capsules is 80-120nm; the preparation method comprises placing porous nanometer fiber matrix of polylactic acid into emulsion of nanometer phase-change capsule, soaking for 15-30min, taking out, and drying to constant weight. The invention can prepare the nano phase-change capsule which has high thermal conductivity and high phase-change latent heat and is easy to disperse, and the nano phase-change capsule is loaded on the polylactic acid porous nanofiber substrate, so that the thermal conductivity and the cooling effect of the substrate are improved; the invention fully utilizes the characteristic that the nano-pore can effectively adsorb small organic molecules and embedded nano-particles, can avoid the defects that the traditional loading method is easy to fall off, the loading process is complex, and a toxic cross-linking agent is possibly used, and has excellent application effect.
Description
Technical Field
The invention belongs to the field of composite material science and technology, and in particular relates to a polylactic acid porous nanofiber-nanometer phase change capsule composite material, and a preparation method and application thereof.
Background
The heating non-burning cigarette consists of a smoking set and a cigarette bullet; when in use, the tobacco cartridges are inserted into the smoking set, and the tobacco cartridges are heated by the smoking set, so that tobacco in the tobacco cartridges is heated and not burnt.
The cigarette bullet part for heating the non-combustible tobacco consists of a filter tip section, a cooling section, an empty pipe section and a tobacco section. The temperature of the tobacco section is 160-200 ℃ when the non-combustible tobacco is heated for smoking, and the temperature of the filter tip section near the lip is 30-40 ℃. At present, domestic heating non-combustion tobacco products are rapidly developed, but a plurality of defects and technical problems to be overcome exist. For example, the smoking taste of domestic heated non-combustible tobacco is lighter than that of traditional cigarettes, the overall length of the cartridge is shorter, and the cooling effect of the cooling section is limited, so that the temperature of the near lip of the filter section is higher.
The nanocapsules are microcapsules with the particle size of 1-1000 nm; the nanocapsule phase-change material is the result of further development of microcapsule (rice) phase-change materials, which not only maintains the technical advantages of microcapsules (when forming microcapsules, the capsule core is coated to be isolated from the external environment, and the properties of the nanocapsule phase-change material can be maintained without influence), but also overcomes the defects of the common microcapsule phase-change materials. The size of the capsule is reduced from micron level to nanometer level, so that the ratio of the surface area to the volume of the capsule is increased, and the heat transfer rate of the phase change material is improved, thereby further expanding the application range of the capsule phase change material; meanwhile, damage caused by collision among particles in use can be greatly reduced. Therefore, in recent years, research on nanocapsule phase-change materials has become a great hotspot.
So far, few reports on the application of nanocapsule phase change materials in heating non-combustible cigarettes are seen.
In view of this, the present invention has been proposed.
Disclosure of Invention
Aiming at the defect of the phase change cooling capacity of the existing heating non-combustion cigarette cooling section material, the invention provides a polylactic acid porous nanofiber-nanometer phase change capsule composite material, and a preparation method and application thereof.
According to one aspect of the invention, a polylactic acid porous nanofiber-nano phase change capsule composite material is provided, and comprises a polylactic acid porous nanofiber matrix and nano phase change capsules attached in nano pores of the polylactic acid porous nanofiber matrix, wherein the pore coverage rate of the polylactic acid porous nanofiber matrix is 15-30%, the average pore size is 180-280nm, and the particle size of the nano phase change capsules is 80-120nm.
In the technical scheme, the polylactic acid porous nanofiber matrix is prepared by adopting an electrostatic spinning method, and comprises the following specific steps:
and dissolving polylactic acid particles in a mixed solvent of dichloromethane and N, N-dimethylacetamide, uniformly mixing, and performing electrostatic spinning as a spinning solution to obtain the polylactic acid porous nanofiber matrix.
Further, in the above technical scheme, in the preparation process of the polylactic acid porous nanofiber matrix, the mass fraction of polylactic acid in the spinning solution is 5-12%.
Specifically, the concentration of polylactic acid affects the result of electrospinning to a large extent; when the concentration of polylactic acid is too low, the entanglement degree of molecular chains in the spinning solution is too small, the jet flow is easy to form a ball in the electrostatic spinning process and cannot be sufficiently drawn, and meanwhile, the jet flow with lower viscosity is more easily stretched and thinned, so that pores are more easily elongated and even stretched to be closed, and the pores in the polylactic acid fiber are greatly reduced; when the concentration of the polylactic acid is too high, the viscosity of the spinning solution is too high, which is not beneficial to the formation of polylactic acid jet flow and the stretching of fibers in the electrostatic spinning process.
Further, in the above technical scheme, in the preparation process of the polylactic acid porous nanofiber matrix, the mass ratio of dichloromethane to N, N dimethylacetamide in the mixed solvent is 5-10:1.
specifically, the pore structure of the surface of the polylactic acid porous nanofiber matrix is greatly influenced by the mass ratio of the mixed solvent of dichloromethane/N, N-dimethylacetamide. In detail, dichloromethane has higher vapor pressure, when the content of dichloromethane in the mixed solvent is low, the solvent volatilization rate of the jet surface in the electrostatic spinning process is relatively low, and the reduction rate and the reduction amplitude of the jet surface temperature are also relatively low; for polylactic acid porous nanofiber which relies on rapid solvent volatilization and temperature change as pore-forming mechanism, the pore density and pore width of the surface of the porous nanofiber are relatively reduced.
Further, in the technical scheme, in the preparation process of the polylactic acid porous nanofiber matrix, the spinning voltage is 10-20kV.
Further, in the technical scheme, in the preparation process of the polylactic acid porous nanofiber matrix, the flow of the spinning solution is 1-2ml/h.
In the technical scheme, the nano phase-change capsule is of a nano composite structure with hexadecanoic acid as a core and silicon dioxide as a shell.
Preferably, in the above technical solution, the nano phase-change capsule is prepared by adopting a miniemulsion method to assist a sol-gel method, and specifically includes:
and (3) dropwise adding the silica sol into the hexadecanoic acid miniemulsion, stirring for 4-8 hours at 65-80 ℃, and cooling to normal temperature to obtain emulsion of the nano phase change capsule.
In detail, the nano phase-change capsule takes liquid with high phase-change latent heat as a core material, and the leakage and the volume change possibly occurring in the phase-change process of the phase-change material are prevented by wrapping the phase-change material around the phase-change material through a wall material with compact structure, and meanwhile, the heat exchange performance of the phase-change material is greatly improved through the introduction of the wall material with high heat conduction performance (such as silicon dioxide); compared with the common micron capsules, the prepared nano phase-change capsules have smaller size, larger surface area, stronger stability, higher high heat conductivity, higher phase-change latent heat and good dispersibility, are easy to load on a substrate with a nano pore structure, and greatly improve the heat conductivity and the phase-change latent heat of the substrate.
Further, in the above technical scheme, in the preparation process of the nano phase-change capsule, the concentration of the silica sol is 0.01-0.03g/ml.
In detail, the silicon dioxide has good thermal conductivity, is safe, nontoxic and low in cost, and can be used as a wall material of the nano phase change capsule to greatly improve the thermal conductivity of the capsule. Specifically, when tetraethyl orthosilicate is used as a precursor for preparing silicon dioxide, the particle size and the particle size distribution of sol particles can be easily controlled by controlling the concentration and the catalysis conditions. In addition, the concentration of the silica sol greatly influences the core material encapsulation effect of the nano phase-change capsule, the size, the stability and the thermal conductivity of the nano phase-change capsule.
Further, in the above technical scheme, in the preparation process of the nano phase-change capsule, the concentration of the hexadecanoic acid miniemulsion is 0.09-0.12g/ml.
In detail, the concentration and emulsification effect of the hexadecanoic acid miniemulsion directly influence the encapsulation effect, the average particle size and the particle size distribution of the nano phase-change capsules; too high a concentration of the hexadecanoic acid miniemulsion easily causes the emulsion to agglomerate, and too low a concentration easily causes the encapsulation rate of the core material and the yield of the nano phase change capsule to be reduced.
Further, in the above technical scheme, in the preparation process of the nano phase-change capsule, the addition volume of the silica sol is 0.6-2.4 times, preferably 1.2 times, of the volume of the hexadecanoic acid miniemulsion.
Further, in the above technical scheme, in the preparation process of the nano phase-change capsule, the stirring speed is 500-800rpm.
Still further, in the above technical scheme, the hexadecanoic acid miniemulsion is prepared by the following method:
adding 9-12g hexadecanoic acid and 0.15-0.22g emulsifier into 100ml water, stirring at 300-1000rpm for 5-20min at 65-75deg.C, homogenizing at 7000-15000rpm for 3-15min to obtain hexadecanoic acid miniemulsion.
Wherein the emulsifier is preferably sodium dodecyl sulfate.
Still further, in the above technical solution, the silica sol is prepared by the following method:
adding 8-12ml of tetraethyl orthosilicate into 90ml of absolute ethyl alcohol, uniformly mixing, adding 30ml of water, regulating the pH value to 9-12 by ammonia water, and stirring for 20-40min to obtain the silica sol.
According to another aspect of the present invention, there is provided a method for preparing the above polylactic acid porous nanofiber-nano phase change capsule composite material, comprising,
and (3) placing the polylactic acid porous nanofiber matrix into emulsion of the nanometer phase change capsule, soaking for 15-30min, taking out, and drying to constant weight.
In the above technical solution, during the impregnation, the stirring speed is controlled to be 10-60rpm.
According to still another aspect of the invention, the application of the polylactic acid porous nanofiber-nanometer phase change capsule composite material in preparing a cooling section of heating non-combustible tobacco is provided.
The invention has the advantages that:
(1) The method provided by the invention can be used for preparing the nano phase-change capsule which has high thermal conductivity and high phase-change latent heat and is easy to disperse, and the nano phase-change capsule is loaded on the polylactic acid porous nanofiber substrate, so that the thermal conductivity and the cooling effect of the substrate are greatly improved;
(2) The method fully utilizes the characteristic that the nano-pores can effectively adsorb organic small molecules and embedded nano particles, adopts an electrostatic spinning method to prepare the superfine polylactic acid porous nano fibers with nano pore structures on the surfaces and the interiors of the fibers, takes the polylactic acid porous nano fibers with a large number of nano pores as a base material, directly and firmly embeds the phase-change nano capsules into the polylactic acid porous nano fiber base material with the nano pore structures through the adsorption action of the nano pores and the interaction of static electricity and functional groups between the base material and the surfaces of the nano capsules by adjusting the nano phase-change capsules to be proper sizes, and can effectively avoid the defects that the traditional micron-sized materials are difficult to directly load on the surfaces of the base material and the micron-sized materials are easy to fall off and the loading process is complex and possibly use of toxic cross-linking agents due to the fact that the traditional micron-sized materials are difficult to be fixed by using adhesive.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to specific examples.
The following examples are given to illustrate the invention but are not intended to limit the scope of the invention, which is defined by the claims.
The experimental reagents, materials, etc. used in the examples of the present invention are commercially available unless otherwise specified.
Unless specifically indicated, the technical means used in the embodiments of the present invention are conventional means well known to those skilled in the art.
Example 1
The invention provides a polylactic acid porous nanofiber-nanometer phase change capsule composite material and a preparation method thereof, and the preparation method comprises the following specific steps:
(1) Dissolving polylactic acid particles in a mass ratio of 8:1, in a mixed solvent of dichloromethane and N, N-dimethylacetamide, uniformly mixing to obtain spinning solution with the mass fraction of 7 percent for later use;
(2) The spinning voltage is 16kV, the flow rate of the spinning solution is 1mL/h, and the polylactic acid porous nanofiber matrix is obtained through electrostatic spinning, the average diameter of the fibers of the prepared polylactic acid porous nanofiber matrix is 1.88 mu m, the pore coverage rate is 24.3%, and the average pore diameter is 256.8nm;
(3) Adding 10g of hexadecanoic acid and 0.20g of sodium dodecyl sulfate into 100ml of water, stirring at 70 ℃ for 15min at 600rpm, and homogenizing at 10000rpm for 8min to obtain hexadecanoic acid miniemulsion;
(4) Adding 10ml of tetraethyl orthosilicate into 90ml of absolute ethyl alcohol, uniformly mixing, adding 30ml of water, regulating the pH value to 11 by using ammonia water, and stirring for 30min to obtain silica sol;
(5) The silica sol prepared in the step (4) is prepared according to the following steps of 1:1 is added into the hexadecanoic acid miniemulsion prepared in the step (3) in a dropwise manner, stirred for 6 hours at the temperature of 70 ℃, and then cooled to normal temperature, so as to obtain emulsion of nano phase-change capsules, wherein the average particle size of the nano phase-change capsules in the prepared emulsion is 102nm, the phase-change latent heat is 122.3kJ/kg, and the heat conductivity coefficient is 0.28W/m.K;
(6) And (3) placing the polylactic acid porous nanofiber matrix prepared in the step (2) into the emulsion of the nano phase-change capsule prepared in the step (5), dipping while slowly stirring (40 rpm), taking out after 20min, and drying to constant weight to obtain the polylactic acid porous nanofiber-nano phase-change capsule composite material.
Finally, folding the prepared polylactic acid porous nanofiber-nanometer phase change capsule composite material into a cylindrical cooling filter section with the diameter of 6mm and the length of 22mm, and simulating and testing the effect of the cylindrical cooling filter section as a heating non-burning cooling section.
Test results show that the prepared cylindrical cooling filter section can well reduce the temperature of the smoke, the temperature of the cooled smoke is about 58 ℃, and the cooling effect is good; and stability is good, and the high temperature flue gas is difficult to take place to adhere and collapse when passing through, and then keeps the smooth circulation of flue gas, and the fragrant smell saturation of flue gas is high, can effectively improve user's suction experience sense.
Example 2
The invention provides a polylactic acid porous nanofiber-nanometer phase change capsule composite material and a preparation method thereof, and the preparation method comprises the following specific steps:
(1) The polylactic acid particles are dissolved in the following mass ratio of 10:1, in a mixed solvent of dichloromethane and N, N-dimethylacetamide, uniformly mixing to obtain spinning solution with the mass fraction of 9 percent for later use;
(2) The spinning voltage is 17.5kV, the flow rate of the spinning solution is 1.2mL/h, and the polylactic acid porous nanofiber matrix is obtained through electrostatic spinning, the average diameter of the fibers of the prepared polylactic acid porous nanofiber matrix is 1.92 mu m, the pore coverage rate is 25.4%, and the average pore diameter is 249.8nm;
(3) Adding 12g of hexadecanoic acid and 0.20g of sodium dodecyl sulfate into 100ml of water, stirring at the speed of 900rpm for 10min at 72 ℃, and homogenizing at the speed of 15000rpm for 5min to obtain hexadecanoic acid miniemulsion;
(4) Adding 12ml of tetraethyl orthosilicate into 90ml of absolute ethyl alcohol, uniformly mixing, adding 30ml of water, regulating the pH value to 12 by using ammonia water, and stirring for 25min to obtain silica sol;
(5) The silica sol prepared in the step (4) is prepared according to the following ratio of 1.2:1 is added into the hexadecanoic acid miniemulsion prepared in the step (3) in a dropwise manner, stirred for 7.5 hours at the temperature of 70 ℃, and then cooled to normal temperature, so as to obtain emulsion of nano phase-change capsules, wherein the average particle size of the nano phase-change capsules in the prepared emulsion is 96nm, the latent heat of phase change is 125.8kJ/kg, and the heat conductivity coefficient is 0.31W/m.K;
(6) And (3) placing the polylactic acid porous nanofiber matrix prepared in the step (2) into the emulsion of the nano phase-change capsule prepared in the step (5), dipping while slowly stirring (40 rpm), taking out after 25min, and drying to constant weight to obtain the polylactic acid porous nanofiber-nano phase-change capsule composite material.
Finally, folding the prepared polylactic acid porous nanofiber-nanometer phase change capsule composite material into a cylindrical cooling filter section with the diameter of 6mm and the length of 22mm, and simulating and testing the effect of the cylindrical cooling filter section as a heating non-burning cooling section.
Test results show that the prepared cylindrical cooling filter section can well reduce the temperature of the smoke, the temperature of the cooled smoke is about 56 ℃, and the cooling effect is good; and stability is good, and the high temperature flue gas is difficult to take place to adhere and collapse when passing through, and then keeps the smooth circulation of flue gas, and the fragrant smell saturation of flue gas is high, can effectively improve user's suction experience sense.
Finally, while the invention has been described in detail with respect to the general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (10)
1. A polylactic acid porous nanofiber-nanometer phase change capsule composite material is characterized in that,
the nano phase-change capsule comprises a polylactic acid porous nanofiber matrix and nano phase-change capsules attached in nano pores of the polylactic acid porous nanofiber matrix, wherein the pore coverage rate of the polylactic acid porous nanofiber matrix is 15-30%, the average pore size is 180-280nm, and the particle size of the nano phase-change capsules is 80-120nm;
the polylactic acid porous nanofiber matrix is prepared by adopting an electrostatic spinning method, and comprises the following specific steps:
dissolving polylactic acid particles in a mixed solvent of dichloromethane and N, N-dimethylacetamide, uniformly mixing and then taking the mixture as a spinning solution to carry out electrostatic spinning to obtain a polylactic acid porous nanofiber matrix;
in the preparation process of the polylactic acid porous nanofiber matrix, the mass fraction of polylactic acid in the spinning solution is 5-12%; in the mixed solvent, the mass ratio of dichloromethane to N, N-dimethylacetamide is 5-10:1, a step of;
the nano phase change capsule is of a nano composite structure with hexadecanoic acid as a core and silicon dioxide as a shell;
the nano phase-change capsule is prepared by adopting a miniemulsion method to assist a sol-gel method, and specifically comprises the following steps:
dropwise adding the silica sol into hexadecanoic acid miniemulsion, stirring for 4-8 hours at 65-80 ℃, and cooling to normal temperature to obtain emulsion of the nano phase change capsule;
in the preparation process of the nano phase-change capsule, the concentration of the silica sol is 0.01-0.03g/ml; the concentration of the hexadecanoic acid miniemulsion is 0.09-0.12g/ml.
2. The polylactic acid porous nanofiber-nano phase change capsule composite material according to claim 1, wherein,
in the preparation process of the polylactic acid porous nanofiber matrix,
the spinning voltage is 10-20kV;
and/or the flow rate of the spinning solution is 1-2ml/h.
3. The polylactic acid porous nanofiber-nano phase change capsule composite material according to claim 1, wherein,
in the preparation process of the nano phase-change capsule,
the added volume of the silica sol is 0.6-2.4 times of the volume of the hexadecanoic acid miniemulsion;
and/or the stirring speed is 500-800rpm.
4. The polylactic acid porous nanofiber-nanophase change capsule composite according to claim 3, wherein the addition volume of the silica sol is 1.2 times the volume of the hexadecanoic acid miniemulsion.
5. The polylactic acid porous nanofiber-nanophase change capsule composite material according to claim 3 or 4, wherein,
the hexadecanoic acid miniemulsion is prepared by the following method:
adding 9-12g hexadecanoic acid and 0.15-0.22g emulsifier into 100ml water, stirring at 300-1000rpm for 5-20min at 65-75deg.C, homogenizing at 7000-15000rpm for 3-15min to obtain hexadecanoic acid miniemulsion.
6. The porous nanofiber-nanofiber phase change nanocomposite capsule composite of claim 5, wherein the emulsifier is sodium dodecyl sulfate.
7. The polylactic acid porous nanofiber-nanophase change capsule composite material according to claim 3 or 4, wherein,
the silica sol is prepared by the following method:
adding 8-12ml of tetraethyl orthosilicate into 90ml of absolute ethyl alcohol, uniformly mixing, adding 30ml of water, regulating the pH value to 9-12 by ammonia water, and stirring for 20-40min to obtain the silica sol.
8. The method for preparing the polylactic acid porous nanofiber-nanometer phase change capsule composite material according to any one of claims 1-7, which is characterized in that,
comprises the steps of placing a polylactic acid porous nanofiber matrix into emulsion of nano phase-change capsules, stirring, soaking for 15-30min, taking out, and drying to constant weight.
9. The method for preparing the polylactic acid porous nanofiber-nanometer phase change capsule composite material according to claim 8, wherein,
during the impregnation, the stirring speed was controlled to be 10-60rpm.
10. Use of the polylactic acid porous nanofiber-nano phase change capsule composite material according to any one of claims 1-7 in preparing a cooling section of heated non-combustible tobacco.
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