CN103205824B - Cyclodextrin supermolecular composite phase-change energy-storage superfine fiber and preparation method and application thereof - Google Patents
Cyclodextrin supermolecular composite phase-change energy-storage superfine fiber and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a cyclodextrin supermolecular composite phase-change energy-storage superfine fiber and a preparation method and application thereof and belongs to the field of functional fiber materials. The cyclodextrin supermolecular composite phase-change energy-storage superfine fiber is prepared by following compositions, by mass, 10-100 parts of cyclodextrin or cyclodextrin derivatives, 20-200 parts of phase change substances and 20-100 parts of cellulose polymer through the electrostatic spinning technology, and can be applied to fields of biomedical materials, separating adsorption materials, energy-saving heat-insulating materials and the like. A supermolecular composite fiber is formed by cyclodextrin and phase-change work components through hydrogen bond and other non-covalent interaction, and the phase change substances are enabled to be less prone to desorption from the cellulose polymer while the obtained energy-storage superfine fiber does not need posttreatment processes like surface crosslinking, so that improvement of heat stability of the materials and simplification of preparation process are facilitated. The main raw materials are natural or seminatural products, so that the cyclodextrin supermolecular composite phase-change energy-storage superfine fiber is good in biocompatibility, nontoxic and harmless, easy to degradation, low in cost and environment-friendly.
Description
Technical field
The invention belongs to functional fibre material field, particularly a kind of cyclodextrin supermolecule composite phase change energy-storing superfine fibre and preparation method thereof and application.
Background technology
Electrostatic spinning (Electrospinning) technology, as a kind of New Processing preparing nano level superfine fiber being different from conventional method, can prepare continuity micron, nanoscale fibrous material easily and efficiently.The diameter of Electrospun can arrive micron, nanoscale, and there is continuity structure and huge specific area, and can be made into variform structure, and electrostatic spinning apparatus is simple, flow process is few, cost is lower and output capacity is higher, and these features make to have broad application prospects based on the functional material of electrostatic spinning technique.On the other hand, phase-changing energy storage material (PCMs:Phase Change Materials) is the material that a class has thermal energy storage and temp regulating function, and temporary transient no energy storage can get up by it, discharges to during needs again, thus the contradiction alleviated between energy supply and demand, economize energy.Being combined with phase-changing energy storage material by electrostatic spinning technique and prepare nanometer, micron order energy-storage fibre material, is a kind of method of preparation of novelty, encapsulation phase-changing energy storage material.Chinese invention patent ZL200610037005.7 discloses a kind of phase-change energy-storage ultra-fine fiber, and this fibrid is made up of different polymer support and phase change material, can keep fiber shape before and after phase transformation, occurs without phase transformation segregation phenomenon.Although this patent solves phase change material and the easy desorption of carrier, leak the problem of oozing out, but the method for its fixing phase change material adopted is immerse in mass fraction 1 ~ 100% cross-linking agent solution after spinning moulding, undertaken surface-crosslinked fixing by the method adding catalyst or ultra violet lamp.This post-processing approach is comparatively complicated.
Cyclodextrin (cyclodextrin, CD), also referred to as ring polydextrose, is by the barrel-like structure of some D-glucopyranose units annular arrangement.In hydrophobic environment in cyclodextrin molecular cavity, lateral surface is hydrophily due to the gathering of hydroxyl.Therefore, cyclodextrin molecular cavity can hold multiple guest molecule formation host-guest inclusion complex compound.In addition, cyclodextrin, as half-natural product, has the features such as nontoxic, good biocompatibility.So the supramolecular materials based on cyclodextrin is widely used in every field.
Summary of the invention
Primary and foremost purpose of the present invention is electrospun fibers manufacturing technology to combine with phase-changing energy storage material, introduce simultaneously and have the cyclodextrin Supramolecular Receptors of binding ability to phase transformation work component in system, a kind of cyclodextrin supermolecule composite phase change energy-storing superfine fibre is provided.
Another object of the present invention is to the preparation method that above-mentioned cyclodextrin supermolecule composite phase change energy-storing superfine fibre is provided.
Another object of the present invention is the application providing above-mentioned cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
Object of the present invention is achieved through the following technical solutions:
A kind of cyclodextrin supermolecule composite phase change energy-storing superfine fibre, be prepared from by electrostatic spinning technique by the component of parts by mass as follows by comprising: cyclodextrin and/or cyclodextrine derivatives 10 ~ 100 parts, phase change material 20 ~ 200 parts, cellulosic polymer 20 ~ 100 parts.First phase change material forms Inclusion Complexes with there being the cyclodextrin acceptor of binding ability to it, is distributed in inside and the surface of fibrous material.
Described cyclodextrin and/or cyclodextrine derivatives are preferably at least one in alpha-cyclodextrin, beta-schardinger dextrin-and gamma-cyclodextrin, permethylated-alpha-cyclodextrin, permethylated-beta-schardinger dextrin-, permethylated-gamma-cyclodextrin, Partially methylatedβ-cyclodextrin, 6-deoxidation-methylol beta-schardinger dextrin-, 6-deoxidation-hydroxyethylβcyclodextrin, 6-deoxidation amino beta-schardinger dextrin-, 6-deoxidation-ethylenediamine beta-schardinger dextrin-and 6-deoxidation-diethylenetriamine beta-schardinger dextrin-.
Described phase change material is preferably polyalcohol and/or LCFA; It is at least one in the polyethylene glycol of 1000 ~ 35000 that described polyalcohol is preferably pentaerythrite, neopentyl glycol, glycerol and weight average molecular weight, and described LCFA is preferably aliphatic acid, as stearic acid and derivative thereof.
Described cellulosic polymer is preferably cellulose and/or cellulose derivative.Described cellulose and/or cellulose derivative are preferably at least one in cellulose, methylcellulose, ethyl cellulose, cyanethyl cellulose, ethyl-cyanoethyl cellulose, cellulose acetate, Carboxymethyl Cellulose, hydroxyethylcellulose, hydroxypropyl cellulose, carboxymethyl cellulose and their derivative thereof.
The diameter of above-mentioned cyclodextrin supermolecule composite phase change energy-storing superfine fibre is 420 ~ 720nm, and enthalpy of phase change scope is between 20 ~ 190J/g, and transition temperature range is 40 ~ 190 DEG C.
The preparation method of above-mentioned cyclodextrin supermolecule composite phase change energy-storing superfine fibre, comprises following steps:
(1) 20 ~ 100 parts by mass of cellulose polymer dissolution are made solution A in solvent; 10 ~ 100 parts by mass cyclodextrin or cyclodextrine derivatives and 20 ~ 200 parts by mass phase change materials are dissolved in solvent and make solution B, stir and make it form cyclic dextrin clathrate complex thing, then add solution A and be uniformly mixed rear formation blend spinning solution.
(2) blend spinning liquid is carried out spinning by high-voltage electrostatic spinning method, obtain superfine fibre.
(3) superfine fibre of gained is carried out drying process, obtain cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
One or more being preferably in water, acetone, ethanol, DMF and DMA of solvent described in step (1) mix.
The mass fraction of the solution A described in step (1) is preferably 5 ~ 20%.
The mass fraction of the solution B described in step (1) is preferably 15 ~ 30%.
The condition of the spinning described in step (2) is preferably: electrospinning voltage is 5 ~ 80kV, distance between spinning head and gathering-device is 5 ~ 50cm, spinning solution sample introduction flow velocity is 0.1 ~ 20mL/h, and ambient temperature is 15 ~ 35 DEG C, and relative air humidity is 30 ~ 90%.
Drying process described in step (3) is preferably in the vacuum drying chamber at 15 ~ 30 DEG C to be carried out.
Above-mentioned cyclodextrin supermolecule composite phase change energy-storing superfine fibre can be applicable to bio-medical material, is separated the field such as sorbing material and energy-saving and heat-insulating material.
The present invention prepares the advantage of continuity super-fine fiber material by electrostatic spinning technique, this a series of large ring acceptor of cyclodextrin is introduced in phase-change energy-storage fibre material, make cyclodextrin and phase transformation work component form supermolecule composite fibre by hydrogen bond and other noncovalent interactions, be conducive to the heat endurance and the simplification post-processing step that improve material.
The present invention has following advantage and effect relative to prior art:
(1) cyclodextrin supermolecule composite phase change energy-storing superfine fibre of the present invention, supramolecular aggregation is formed by the molecular linkage ability of the phase-change accumulation energy work component of cyclodextrin, make gained energy-storage ultra-fine fiber can make phase change material not easily desorption from cellulosic polymer carrier without the need to the surface-crosslinked last handling process that waits, while in conjunction with solid-liquid and solid-solid phase transition material advantage, simplify the preparation process of such superfine fibre.
(2) cyclodextrin supermolecule composite phase change energy-storing superfine fibre of the present invention comparatively prior art, has better heat endurance, and preparation process is simple, without the need to changing existing spinning solution preparation technology.
(3) cyclodextrin supermolecule composite phase change energy-storing superfine fibre of the present invention is environmental friendly product, and the main raw material cyclodextrin selected is half-natural product, and good biocompatibility is nontoxic, easily degrades.Selected cellulosic polymer carrier is also natural or half-natural product, wide material sources, with low cost, asepsis environment-protecting.Selected phase change material is also nontoxic.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) cellulose acetate (CA, number-average molecular weight 30000, degree of substitution with acetyl group 2.5) of 100 parts by mass is dissolved in the mixed solvent that acetone and DMF prepare with mass ratio 1:1 and makes the solution that mass fraction is 15%; By water-soluble for the PEG-4000 of the alpha-cyclodextrin of 30 parts by mass and 100 parts by mass and N, the solution that mass fraction is 15% is made in the mixed solvent that dinethylformamide coordinates with mass ratio 1:1, mechanical agitation 2h makes it form cyclic dextrin clathrate complex thing, then adds cellulose acetate solution mechanical agitation and evenly form blend spinning liquid.
(2) loading of blend spinning liquid is carried out spinning with in the fluid reservoir of spinning head by high-voltage electrostatic spinning method, obtain superfine fibre; The condition of spinning is: ambient temperature is 25 DEG C, relative humidity 90%, and electrospinning voltage is 80kV, and the distance between spinning head and collecting board is 50cm, and spinning solution sample introduction flow velocity is 0.5mL/h.
(3) superfine fibre of gained is put into 25 DEG C of vacuum drying chambers and carry out drying process, obtain cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
(4) ESEM records this superfine fibre average diameter is 420nm, and by differential scanning calorimetry (DSC) test, enthalpy of phase change is 109.7J/g, and phase transition temperature is 59.6 DEG C.
Embodiment 2
(1) hydroxypropyl cellulose (Hydroxypropylcelliloxe, number-average molecular weight 80000) of 100 parts by mass is dissolved in the mixed solvent that ethanol and water prepares with mass ratio 5:1 and makes the solution that mass fraction is 10%; By water-soluble for the PEG-6000 0 of the beta-schardinger dextrin-of 10 parts by mass and 20 parts by mass and N, the solution that mass fraction is 15% is made in the mixed solvent that N-dimethylacetylamide coordinates with mass ratio 1:1, mechanical agitation 2h makes it form cyclic dextrin clathrate complex thing, then adds hydroxypropyl cellulose solution mechanical agitation and evenly form blend spinning liquid.
(2) loading of blend spinning liquid is carried out spinning with in the fluid reservoir of spinning head by high-voltage electrostatic spinning method, obtain superfine fibre; The condition of spinning is: ambient temperature is 35 DEG C, relative humidity 30%, and electrospinning voltage is 5kV, and the distance between spinning head and collecting board is 5cm, and spinning solution sample introduction flow velocity is 0.1mL/h.
(3) superfine fibre of gained is put into 15 DEG C of vacuum drying chambers and carry out drying process, obtain cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
(4) ESEM records this superfine fibre average diameter is 580nm, and by differential scanning calorimetry (DSC) test, enthalpy of phase change is 24.5J/g, and phase transition temperature is 53.2 DEG C.
Embodiment 3
(1) hydroxyethylmethyl-cellulose (molecular weight 40000) of 20 parts by mass is dissolved in the mixed solvent that ethanol and DMF prepare with mass ratio 1:1 and makes the solution that mass fraction is 5%; By the β-permethylated beta-cyclodextrin of 100 parts by mass and the pentaerythrite of 200 parts by mass is water-soluble and N, the solution that mass fraction is 20% is made in the mixed solvent that dinethylformamide coordinates with mass ratio 3:1, mechanical agitation 2h makes it form cyclic dextrin clathrate complex thing, then adds hydroxyethylmethyl-cellulose solution movement and stir and form blend spinning liquid.
(2) loading of blend spinning liquid is carried out spinning with in the fluid reservoir of spinning head by high-voltage electrostatic spinning method, obtain superfine fibre; The condition of spinning is: ambient temperature is 15 DEG C, relative humidity 55%, and electrospinning voltage is 10kV, and the distance between spinning head and collecting board is 20cm, and spinning solution sample introduction flow velocity is 1.0mL/h.
(3) superfine fibre of gained is put into 25 DEG C of vacuum drying chambers and carry out drying process, obtain cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
(4) ESEM records this superfine fibre average diameter is 690nm, and by differential scanning calorimetry (DSC) test, enthalpy of phase change is 186.4J/g, and phase transition temperature is 187.9 DEG C.
Embodiment 4
(1) carboxymethyl cellulose (molecular weight 20000) of 50 parts by mass is dissolved in the mixed solvent that acetone and water prepares with mass ratio 4:1 and makes the solution that mass fraction is 20%; By water-soluble for the stearic acid of the 6-of 50 parts by mass deoxidation-hydroxyethylβcyclodextrin and 100 parts by mass and N, the solution that mass fraction is 30% is made in the mixed solvent that N-dimethylacetylamide coordinates with mass ratio 2:1, mechanical agitation 2h makes it form cyclic dextrin clathrate complex thing, then adds hydroxymethyl cellulose solution mechanical agitation and evenly form blend spinning liquid.
(2) loading of blend spinning liquid is carried out spinning with in the fluid reservoir of spinning head by high-voltage electrostatic spinning method, obtain superfine fibre; The condition of spinning is: ambient temperature is 21 DEG C, relative humidity 45%, and electrospinning voltage is 12kV, and the distance between spinning head and collecting board is 15cm, and spinning solution sample introduction flow velocity is 1.5mL/h.
(3) superfine fibre of gained is put into 30 DEG C of vacuum drying chambers and carry out drying process, obtain cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
(4) ESEM records this superfine fibre average diameter is 450nm, and by differential scanning calorimetry (DSC) test, enthalpy of phase change is 112.9J/g, and phase transition temperature is 71.3 DEG C.
Embodiment 5
(1) cellulose acetate of 70 parts by mass (CA belongs to average molecular weight 30000, degree of substitution with acetyl group 2.5) is dissolved in the mixed solvent that acetone and DMF prepare with mass ratio 1:1 and makes the solution that mass fraction is 15%; The solution that mass fraction is 30% is made in the mixed solvent water-soluble to the β-RAMEB of 100 parts by mass and the neopentyl glycol of 100 parts by mass and ethanol coordinated with mass ratio 1:1, mechanical agitation 2h makes it form cyclic dextrin clathrate complex thing, then adds cellulose acetate solution mechanical agitation and evenly form blend spinning liquid.
(2) loading of blend spinning liquid is carried out spinning with in the fluid reservoir of spinning head by high-voltage electrostatic spinning method, obtain superfine fibre; The condition of spinning is: ambient temperature is 30 DEG C, relative humidity 70%, and electrospinning voltage is 25kV, and the distance between spinning head and collecting board is 20cm, and spinning solution sample introduction flow velocity is 20mL/h.
(3) superfine fibre of gained is put into 25 DEG C of vacuum drying chambers and carry out drying process, obtain cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
(4) ESEM records this superfine fibre average diameter is 720nm, and by differential scanning calorimetry (DSC) test, enthalpy of phase change is 65.9J/g, and phase transition temperature is 45.6 DEG C.
Comparative example 1
(1) cellulose acetate of 100 parts by mass (CA belongs to average molecular weight 30000, degree of substitution with acetyl group 2.5) is dissolved in the mixed solvent that acetone and DMF prepare with mass ratio 1:1 and makes the solution that mass fraction is 15%; The solution that mass fraction is 15% is made in the mixed solvent water-soluble for the PEG-4000 of 100 parts by mass and DMF coordinated with mass ratio 1:1; Above-mentioned two kinds of solution movement are stirred and forms blend spinning liquid.
(2) loading of blend spinning liquid is carried out spinning with in the fluid reservoir of spinning head by high-voltage electrostatic spinning method, obtain superfine fibre; The condition of spinning is: ambient temperature is 25 DEG C, relative humidity 90%, and electrospinning voltage is 80kV, and the distance between spinning head and collecting board is 50cm, and spinning solution sample introduction flow velocity is 0.5mL/h.
(3) superfine fibre of gained is put into 25 DEG C of vacuum drying chambers and carry out drying process, obtain cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
(4) ESEM records this superfine fibre average diameter is 360nm, and by differential scanning calorimetry (DSC) test, enthalpy of phase change is 85.6J/g, and phase transition temperature is 55.7 DEG C.
The average diameter of the cyclodextrin supermolecule composite phase change energy-storing superfine fibre that above-described embodiment prepares, phase transition temperature and enthalpy of phase change are as shown in table 1:
Table 1
| Average diameter/nm | Enthalpy of phase change/J/g | Phase transition temperature/DEG C | |
| Embodiment 1 | 420 | 109.7 | 59.6 |
| Comparative example 1 | 360 | 85.6 | 55.7 |
| Embodiment 2 | 580 | 24.5 | 53.2 |
| Embodiment 3 | 690 | 186.4 | 187.9 |
| Embodiment 4 | 450 | 112.9 | 71.3 |
| Embodiment 5 | 720 | 659 | 456 |
Result shows: cyclodextrin supermolecule composite phase change energy-storing superfine fibre average diameter prepared by the present invention is between 420 ~ 720nm, illustrate that this cyclodextrin supermolecule composite phase change energy-storing superfine fibre has nanometer, micron-sized mesostructure, enthalpy of phase change scope is between 24.5 DEG C ~ 186.4J/g, phase transition temperature is between 45.6 ~ 187.9 DEG C, illustrate this cyclodextrin supermolecule composite phase change energy-storing superfine fibre be applicable to multiple environment temperature under energy-storage thermal-insulating needs.By comparing of embodiment 1 and comparative example 1: under equal process conditions, cyclodextrin supermolecule composite phase change energy-storing superfine fibre has higher enthalpy of phase change, illustrates that this fiber has better insulating power.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. a cyclodextrin supermolecule composite phase change energy-storing superfine fibre, it is characterized in that being prepared from by electrostatic spinning technique by the component of parts by mass as follows by comprising: cyclodextrin and/or cyclodextrine derivatives 10 ~ 100 parts, phase change material 20 ~ 200 parts, cellulosic polymer 20 ~ 100 parts;
Described phase change material is polyalcohol and/or LCFA;
Described cyclodextrin and/or cyclodextrine derivatives are at least one in alpha-cyclodextrin, beta-schardinger dextrin-and gamma-cyclodextrin, permethylated-alpha-cyclodextrin, permethylated-beta-schardinger dextrin-, permethylated-gamma-cyclodextrin, Partially methylatedβ-cyclodextrin, 6-deoxidation-methylol beta-schardinger dextrin-, 6-deoxidation-hydroxyethylβcyclodextrin, 6-deoxidation amino beta-schardinger dextrin-, 6-deoxidation-ethylenediamine beta-schardinger dextrin-and 6-deoxidation-diethylenetriamine beta-schardinger dextrin-.
2. cyclodextrin supermolecule composite phase change energy-storing superfine fibre according to claim 1, is characterized in that: described cellulosic polymer is cellulose and/or cellulose derivative.
3. cyclodextrin supermolecule composite phase change energy-storing superfine fibre according to claim 2, is characterized in that: the described polyalcohol at least one that to be pentaerythrite, neopentyl glycol, glycerol and weight average molecular weight be in the polyethylene glycol of 1000 ~ 35000; Described LCFA is aliphatic acid; Described cellulose and/or cellulose derivative are at least one in cellulose, methylcellulose, ethyl cellulose, cyanethyl cellulose, ethyl-cyanoethyl cellulose, cellulose acetate, Carboxymethyl Cellulose, hydroxyethylcellulose, hydroxypropyl cellulose and carboxymethyl cellulose.
4. the cyclodextrin supermolecule composite phase change energy-storing superfine fibre according to any one of claims 1 to 3, it is characterized in that: the diameter of described cyclodextrin supermolecule composite phase change energy-storing superfine fibre is 420 ~ 720nm, enthalpy of phase change scope is between 20 ~ 190J/g, and transition temperature range is 40 ~ 190 DEG C.
5. the preparation method of the cyclodextrin supermolecule composite phase change energy-storing superfine fibre described in any one of claims 1 to 3, is characterized in that comprising following steps:
(1) 20 ~ 100 parts by mass of cellulose polymer dissolution are made solution A in solvent; 10 ~ 100 parts by mass cyclodextrin or cyclodextrine derivatives and 20 ~ 200 parts by mass phase change materials are dissolved in solvent and make solution B, stir and make it form cyclic dextrin clathrate complex thing, then add solution A and be uniformly mixed rear formation blend spinning solution;
(2) blend spinning liquid is carried out spinning by high-voltage electrostatic spinning method, obtain superfine fibre;
(3) superfine fibre of gained is carried out drying process, obtain cyclodextrin supermolecule composite phase change energy-storing superfine fibre.
6. the preparation method of cyclodextrin supermolecule composite phase change energy-storing superfine fibre according to claim 5, is characterized in that:
Solvent described in step (1) is that one or more in water, acetone, ethanol, DMF and DMA mix;
The mass fraction of the solution A described in step (1) is 5 ~ 20%;
The mass fraction of the solution B described in step (1) is 15 ~ 30%.
7. the preparation method of cyclodextrin supermolecule composite phase change energy-storing superfine fibre according to claim 5, is characterized in that:
The condition of the spinning described in step (2) is: electrospinning voltage is 5 ~ 80kV, distance between spinning head and gathering-device is 5 ~ 50cm, spinning solution sample introduction flow velocity is 0.1 ~ 20mL/h, and ambient temperature is 15 ~ 35 DEG C, and relative air humidity is 30 ~ 90%.
8. the preparation method of cyclodextrin supermolecule composite phase change energy-storing superfine fibre according to claim 5, is characterized in that:
Drying described in step (3) is treated in the vacuum drying chamber at 15 ~ 30 DEG C to be carried out.
9. the cyclodextrin supermolecule composite phase change energy-storing superfine fibre described in any one of claims 1 to 3 is in bio-medical material, the application be separated in sorbing material and energy-saving and heat-insulating material field.
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| CN105040279B (en) * | 2015-08-14 | 2017-05-03 | 北京化工大学 | Preparation method for core-shell structure nanofiber membrane with cyclodextrinpolypseudortaxane molecule channel on surface |
| CN106498626A (en) * | 2016-10-31 | 2017-03-15 | 天津农学院 | A kind of preparation method of cross linked ciclodextrines nano fibrous membrane |
| CN109054765B (en) * | 2018-08-22 | 2021-01-01 | 南京林业大学 | Polyethylene glycol/ethyl cellulose phase change microcapsule and preparation method thereof |
| CN113062003B (en) * | 2021-04-13 | 2022-12-20 | 浙江理工大学 | Method for preparing high latent heat nanometer intelligent fiber through crosslinking |
| CN114874756B (en) * | 2022-07-12 | 2022-09-16 | 北京金羽新能科技有限公司 | Composite phase change material and preparation method and application thereof |
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