CN108929629A - A kind of preparation method of phase transformation Infrared stealthy materials - Google Patents
A kind of preparation method of phase transformation Infrared stealthy materials Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/004—Reflecting paints; Signal paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/085—Copper
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Abstract
The invention discloses a kind of preparation methods of phase transformation Infrared stealthy materials, after collagenous fibres being dispersed with stirring in suitable organic solution uniformly, it is formed through filtering, uniform phase-change material is added dropwise, the phase-change material compound with collagenous fibres base can be obtained after drying in the shade naturally.Or by collagenous fibres after suitable organic solvent is dispersed with stirring uniformly, is formed through filtering, uniform phase-change material is added dropwise, after drying in the shade naturally, in its top finishing metal powder M coating or oxide M OxThe phase-change material compound with collagenous fibres base can be obtained in thermal insulation layer.The present invention can be effectively prevented the leakage after phase-change material phase transformation, adsorption group is obtained without artificially carrying out chemical graft again, manufacturing cycle is shortened, improves production efficiency, reduce preparation cost, it is thus also avoided that the prior art uses problems brought by surfactant and catalyst.
Description
Technical field
The invention belongs to the research fields of phase-change material, and in particular to a kind of to utilize the distinctive multi-layer fiber of collagenous fibres
Structure and chemical reaction characteristic are come the method for preparing phase-change material, and its application in infrared stealth field.
Background technique
Phase-change material mainly utilizes (cold) amount of heat of phase transition process absorption environment, and if necessary to Environment release heat
(cold) amount, with this be controlled material and ambient enviroment temperature [Li Faxue, Zhang Guangping, Wu Lili, it is remaining to build brave phase-change material
Textile journal, 2003,24,167-169. are applied on new infrared camouflage clothes].Wherein, solid-liquid phase change material is because of its phase
The advantages that larger, volume change is smaller, transition temperature range is wide, moderate strength, is melted in heating, becomes and studies more material at present.
Solid-liquid phase change material is usually prepared by solid-liquid phase change material after phase transformation the problems such as bring leakage, corrosion in order to prevent
Polymerization macromolecule material as wall material phase-change material be capsule-core hud typed microcapsules come using [Yang Aidi, Wang Zhihui, Zhang Cun,
The research modern defense technology of equal thermal infrared cooling-phase transformation multiplex stealth coating, Lee 2009,5,21-24. lack bright, Jing Wenbin,
Xu Liang, Wang Lixi, the preparation and representation functional material of its soil infrared stealth paraffin microcapsule, 2013,44,1034-
1038.].But the preparation of this microcapsules is extremely stringent to the selection of wall material, and the presence of wall material will weaken heat transfer, no
Temperature is made conducive to phase-change material and timely being responded.In addition, its preparation process is complicated, condition is harsh, and microcapsule stability
It is poor.
It is proposed in order to solve the above problem using porous matrix material come adsorption storage phase-change material, is prepared compound in recent years
Method [Wu Zimin, Huang Xue, the progress Zhong Kai agriculture of the porous base sizing phase-change material of Cui Yingde, Feng Guang wick of phase-change material
Industrial engineering (IE) institute journal, 2015,28,66-70.].Such material can prevent phase-change material leak and etching problem, and it is porous
Matrix can thennal conduction enhancement process significantly, shorten phase-change material transformation time, to timely respond to the variation of environment temperature.Closely
Over year there are mainly four types of the more porous matrix of domestic and international application: expanded graphite matrix, expanded perlite matrix, porous ceramic matrix
Body and the porous metal matrix [system of the porous base composite phase-change material of Chen Limeng, Zhu Xiaoqin, Zhou Xintao, Hu Jing, Lan Yang, Chang Jinghua
It is standby with progress material Leader, 2016,30,127-132.].But the porous base composite phase-change of these porous matrix preparation
The extensive use of material still has problems, as the loose porous vermicular texture of expanded graphite matrix mechanical strength compared with
Difference, pore-size distribution are uneven；Expanded perlite matrix thermal coefficient is small；Porous metal matrix has stronger thermal conductivity, still
Alternative porous metal matrix is less, and its chemical stability is very poor.At present, it would be highly desirable to develop novel storage substrate material
Material is used to prepare composite phase-change material.
Summary of the invention
The purpose of the invention patent is to be directed to the deficiency of existing product and provide a kind of using natural collagen fibre as substrate storage
Deposit phase-change material preparation fiber base composite phase-change material.Its main feature is that using collagenous fiber material caused by leather industry as
Substrate, the good fiber base composite phase-change material of production chemical stability, and it is applied to Infrared stealthy materials field.
In order to achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of phase transformation Infrared stealthy materials the following steps are included:
(1) collagenous fibres are dispersed with stirring in suitable organic solution uniformly；
(2) it is formed through filtering；
(3) uniform phase-change material is added dropwise；
(4) the phase-change material Fiber/P compound with collagenous fibres base can be obtained after drying in the shade naturally；
Or,
Naturally after drying in the shade, with organic bond on it top finishing metal powder M reflection layer or its lower surface cover with paint, lacquer, colour wash, etc. aoxidize
Object MOxThe phase-change material Fiber/P/M or MO compound with collagenous fibres base can be obtained in thermal insulation layerx/Fiber/P。
Further, the collagenous fibres are using ox-hide, sheepskin or pigskin as the raw material fibre that routinely method for leather-making produces
Dimension.
Further, the phase-change material and collagenous fibres mass ratio are 1~2:1.
Further, the phase-change material is paraffin.
Further, the paraffin and collagenous fibres mass ratio are 2:1.
Further, the organic solution is dehydrated alcohol, PDMS solution (2wt%, dodecane are solvent), plant polyphenol
Any one in solution.
Further, powder used is wicker copper (Cu@Ag) or WO in the metal powder M reflection coating3In (≤5 μm)
One kind, the organic bond be PDMS (50wt%, dodecane are solvent).
Further, the oxide M Ox thermal insulation layer is the SiO with 100nm2As heat-insulated oxide, PDMS
(50wt%, dodecane are solvent) is used as organic bond.
Further, the paraffin and collagenous fibres mass ratio are 1~2:1.
It is worth noting that the collagenous fibres based phase-change material prepared in above-mentioned technical proposal is met the tendency of in infrared stealth field
When, oxide heat insulation layer is contacted with target surface, and metal-powder coating is contacted as superficial layer with air.
Compared with prior art, the present invention it has the positive effect that:
1, natural collagen fibre is mainly the microfibril being self-assembly of by tropocollagen molecule, and multiple microfibrils further assemble
Nanofibrils are formed, nanofibrils are then assembled into bundles of nanofibers, and bundles of nanofibers is finally assembled into the glue of micro-meter scale
Fibrinogen beam (5~10 μm of diameter), the collagen for being knitted to form high-sequential between collagenous fiber bundle in a particular manner again are fine
Tie up net.It follows that collagenous fibres base is a kind of solid fiber material with higher porosity, it is this unique across nanometer
The porous structure of scale to micro-meter scale provides good structure basis for adsorption storage phase-change material；
2, contain a large amount of hydrophobic region in the tropocollagen molecule of collagenous fibres, it is adsorbable to store a large amount of phase-change material, and effectively
Ground prevents the leakage after phase-change material phase transformation, obtains adsorption group without artificially carrying out chemical graft again, thus not only shortens
Manufacturing cycle, improves production efficiency, reduces preparation cost, it is thus also avoided that the prior art uses surfactant and catalysis
Problems brought by agent；
3, after collagenous fibres are impregnated by organic solution, hydrophobicity is greatly enhanced, and is conducive to phase-change material paraffin inside it
It is uniformly distributed, and is leaked after preventing paraffin from undergoing phase transition；
4, collagenous fibres contain a large amount of moisture (being greater than 12%).The specific heat capacity of water is big, and it is larger that this has collagenous fibres
Thermal capacity, it is thus possible to after absorbing a large amount of infrared emanations, temperature is not increased significantly, and it is excellent that this is conducive to processability
Infrared stealthy materials；
5, oxide heat insulation layer can effectively delay or obstruct the heat that high-temperature targets are conducted to collagenous fibres based phase-change material, into
One step delays the raising of collagenous fibres based phase-change material temperature, improves the infrared stealth effect of high-temperature targets；
6, the metal powder in metal powder reflecting layer is to infrared light high reflectance, low absorptivity, therefore it is coated on to collagen fibre
When Wiki phase-change material surface, the infrared emanation of external environment is reflected, and is effectively reduced collagenous fibres based phase-change material
Surface infrared emittance realize the infrared stealth of itself to reduce the infrared intensity of collagenous fibres based phase-change material；
7, natural leather is a kind of high molecular material from a wealth of sources mainly from the skin of the animals such as ox, sheep, pig.
Detailed description of the invention
SiO prepared by Fig. 1 embodiment 12The DSC of/Fiber/P/Cu@Ag schemes；
SiO prepared by Fig. 2 embodiment 12The temperature that/Fiber/P/Cu@Ag is placed in 40 DEG C of heating plates changes with time song
Line；
The DSC of Fiber/P/Cu@Ag prepared by Fig. 3 embodiment 2 schemes；
Fiber/P/Cu@Ag prepared by Fig. 4 infrared detecting set testing example 2 is placed in the temperature in 40 DEG C of heating plates at any time
Change curve；
The DSC of Fiber/P prepared by Fig. 5 embodiment 3 schemes；
Fiber/P prepared by Fig. 6 embodiment 3 is placed in the temperature versus time curve in 40 DEG C of heating plates；
The DSC of Fiber/P prepared by Fig. 7 embodiment 4 schemes；
Fiber/P prepared by Fig. 8 embodiment 4 is placed in the temperature versus time curve in 40 DEG C of heating plates；
Fiber/P/WO prepared by Fig. 9 embodiment 53DSC figure；
Fiber/P/WO prepared by Figure 10 embodiment 53The temperature versus time curve being placed in 40 DEG C of heating plates；
The DSC of Fiber/P/Cu@Ag prepared by Figure 11 embodiment 6 schemes；
Fiber/P/Cu@Ag prepared by Figure 12 embodiment 6 is placed in the temperature versus time curve in 40 DEG C of heating plates；
The DSC of Fiber/P prepared by Figure 13 embodiment 7 schemes；
Fiber/P prepared by Figure 14 embodiment 7 is placed in the temperature versus time curve in 40 DEG C of heating plates.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that the present embodiment is served only for
Invention is further explained, but the contents of the present invention are not limited only to content involved in embodiment, should not be understood as
Limiting the scope of the invention, the person skilled in the art in the field can make some non-according to the content of aforementioned present invention
The modifications and adaptations of essence.
Embodiment 1
4g chromium-containing collagen fiber Fiber is stirred in 200ml PDMS solution (2wt%, dodecane are solvent) at room temperature
It after mixing 30min, filters and forms a film and drop evenly 8g vasoliniment (P), by its upper surface after collagenous fibres dry in the shade solidification naturally
Cover with paint, lacquer, colour wash, etc. the reflecting layer@Ag wicker copper Cu and Nano-meter SiO_2 respectively with lower surface2Thermal insulation layer.The reflecting layer Cu@Ag is 0.8g PDMS solution
The mixture of (50wt%, dodecane are solvent) and 2g Cu@Ag；Nano-meter SiO_22Thermal insulation layer be 0.8g PDMS solution (50wt%,
Dodecane is solvent) and 2g Nano-meter SiO_22Mixture.Collagenous fibres base composite phase-change material is obtained after to be dried to obtain
Chromium-containing collagen fiber base composite phase-change material SiO2/Fiber/P/Cu@Ag.Through known to DSC test (Fig. 1), the present embodiment is made
Standby SiO2There is endothermic peak at~31 DEG C in/Fiber/P/Cu@Ag, and~23 DEG C exothermic peak occur.Fig. 2 is SiO2/Fiber/P/
Cu@Ag is covered on 40 DEG C of high-temperature heating plates, and the versus time curve of its surface temperature is observed by infrared thermoviewer.By
Figure is it is found that after 20min, SiO2/ Fiber/P/Cu@Ag temperature is stablized at~19 DEG C.In summary, SiO2/Fiber/P/
When Cu@Ag covering high-temperature target, a large amount of heat can be lost by the way that phase transition occurs, slow down the raising of own temperature, inhibit high
The infrared emanation intensity of warm target surface makes high-temperature targets realize infrared stealth.
Embodiment 2
4g chromium-containing collagen fiber Fiber is stirred in 200ml PDMS solution (2wt%, dodecane are solvent) at room temperature
After mixing 30min, filters to form a film and simultaneously drop evenly 8g vasoliniment (P), after collagenous fibres dry in the shade solidification naturally, surface on it
Cover with paint, lacquer, colour wash, etc. Cu@Ag coating.Cu@Ag coating is made of 0.8g PDMS solution (50wt%, dodecane are solvent) and 2g Cu@Ag.
Chromium-containing collagen fiber base composite phase-change material Fiber/P/Cu Ag is obtained after to be dried and natural cooling.Through known to DSC test
There is endothermic peak and exothermic peak with~24 DEG C at~31 DEG C respectively in (Fig. 3), Fiber/P/Cu@Ag prepared by the present embodiment.When
Fiber/P/Cu@Ag is covered on 40 DEG C of high-temperature heating plates, and the change at any time of its surface temperature is observed by infrared thermoviewer
Change curve, as shown in Figure 4.After 30min, slowly increasing occurs in Fiber/P/Cu@Ag temperature, and stablizes after 60min
~22 DEG C.It in summary, can be by the way that a large amount of heat of phase transition loss occurs when Fiber/P/Cu@Ag covering high-temperature target surface
Amount slows down the raising of own temperature, reduces the infrared emanation intensity on high-temperature targets surface, reduces in the infrared of its ambient enviroment
The difference of heat radiation realizes good infrared stealth effect.
Embodiment 3
4g chromium-containing collagen fiber Fiber is stirred in 200ml PDMS solution (2wt%, dodecane are solvent) at room temperature
It after mixing 30min, filters and forms a film and uniformly drip 8g vasoliniment (P), obtain glue containing chromium after collagenous fibres dry in the shade solidification naturally
Fibrinogen base composite phase-change material Fiber/P.Through known to DSC test (Fig. 5), Fiber/P prepared by the present embodiment is~35
DEG C there is apparent endothermic peak, exothermic peak occurs at~28 DEG C.Thus speculate, when Fiber/P is covered in high-temperature targets surface,
A large amount of heat can be lost by the way that phase transition occurs in Fiber/P, to slow down the raising of own temperature, reduce high-temperature targets and (add
Hot plate) surface temperature.As shown in fig. 6, when Fiber/P is covered in 40 DEG C of heater plate surfaces, after 10min, Fiber/P
Slowly increasing occurs in temperature, and~24 DEG C are risen to after 60min.Therefore, the Fiber/P for being covered in high-temperature targets surface can lead to
It crosses generation phase transition and a large amount of heat is lost, inhibit the infrared emanation intensity on high-temperature targets surface, realize good infrared hidden
Body effect.
Embodiment 4
4g collagenous fibres are stirred into 30min in 200ml PDMS solution (2wt%, dodecane are solvent) at room temperature
Afterwards, it filters and forms a film and uniformly drip 4g vasoliniment (P), it is compound to obtain collagenous fibres base after collagenous fibres dry in the shade solidification naturally
Phase-change material Fiber/P.Through known to DSC test (Fig. 7), there is endothermic peak in~31 DEG C in Fiber/P prepared by the present embodiment,
There is exothermic peak in~27 DEG C.Therefore, Fiber/P can occur phase transition loss or discharge a large amount of heat, slow down own temperature
Be raised and lowered.Fig. 8 is that Fiber/P is covered on 40 DEG C of high-temperature heating plates, observes its surface temperature by infrared thermoviewer
Versus time curve.As seen from the figure, after 20min, slowly increasing occurs in Fiber/P surface temperature, and in 60min
After rise to~26 DEG C.In conclusion a large amount of heat can be absorbed by the way that phase transition occurs when Fiber/P covering high-temperature target,
But own temperature will not increase, to inhibit the infrared emanation intensity on high-temperature targets surface, achieve good infrared hidden
Body effect.
Embodiment 5
The stirring in 200ml PDMS solution (2wt%, dodecane are solvent) at room temperature by 4g collagenous fibres Fiber
30min drops evenly 8g vasoliniment (P) after filtering molding, after collagenous fibres dry in the shade solidification naturally, top finishing on it
Receive WO3Coating.WO3Coating is by 1.6g PDMS solution (50wt%, dodecane are solvent) and 4g WO3Composition.It is to be dried and from
So collagenous fibres base composite phase-change material Fiber/P/WO is obtained after cooling3.(Fig. 9) is known through DSC test, the present embodiment institute
The Fiber/P/WO of preparation3There is endothermic peak at~32 DEG C, exothermic peak occurs at~12 and 24 DEG C.Therefore, Fiber/P/WO3It can
Effectively slow down being raised and lowered for its own temperature by absorbing or discharging heat.Figure 10 is Fiber/P/WO3It is covered in
On 40 DEG C of high-temperature heating plates, the versus time curve of its surface temperature is observed by infrared thermoviewer.As seen from the figure, pass through
After 40min, Fiber/P/WO3Slowly increasing occurs in temperature, and stablizes after 60min to~28 DEG C.It follows that Fiber/P/
WO3When covering high-temperature target, a large amount of heat can be absorbed by the way that phase transition occurs, slow down the raising of own temperature, to inhibit
The infrared emanation intensity on high-temperature targets surface realizes good infrared stealth effect.
Embodiment 6
The stirring in 200ml PDMS solution (2wt%, dodecane are solvent) at room temperature by 4g collagenous fibres Fiber
30min drops evenly 8g vasoliniment (P) after filtering molding, after collagenous fibres dry in the shade solidification naturally, top finishing on it
Cu@Ag coating.Cu@Ag coating is the mixture of the PDMS (50wt%) and 2g Cu@Ag of 1.6g.After dry and natural cooling
Obtain collagenous fibres base composite phase-change material Fiber/P/Cu Ag.Known to DSC test (Figure 11), prepared by the present embodiment
There is endothermic peak at~28 DEG C in Fiber/P/Cu@Ag, and~12 exothermic peak occur with~25 DEG C.Therefore, Fiber/P/Cu@Ag can lead to
It crosses and absorbs or discharge heat to delay the variation (being raised and lowered) of own temperature.Figure 12 is that Fiber/P/Cu@Ag is covered in 40
DEG C high-temperature heating plate on, the versus time curve of its surface temperature is observed by infrared thermoviewer.As seen from the figure, pass through
After 20min, slowly increasing occurs in Fiber/P/Cu@Ag temperature, and stablizes after 60min to~21 DEG C.It follows that Fiber/
When P/Cu@Ag covering high-temperature target, a large amount of heat can be absorbed by the way that phase transition occurs, slow down the raising of own temperature, inhibit
The infrared emanation intensity on high-temperature targets surface realizes good infrared stealth effect.
Embodiment 7
4g collagenous fibres Fiber and 0.12g BT are dispersed into 30min in 100ml deionized water at room temperature, 4g collagen is added
Fiber and 100ml dehydrated alcohol are simultaneously warming up to 35 DEG C, stirring 1h.It filters and forms a film and drop evenly 6g vasoliniment, to collagen fibre
Dimension nature dry in the shade solidification after obtain collagenous fibres base composite phase-change material Fiber/P.(Figure 13) is known through DSC test, this reality
It applies Fiber/P prepared by example and endothermic peak occurs at~31 DEG C ,~23 DEG C exothermic peak occur.Therefore Fiber/P can pass through absorption
Or heat is discharged to regulate and control the variation of own temperature.Figure 14 be Fiber/P be covered on 40 DEG C of high-temperature heating plates, by it is infrared at
As instrument observes the versus time curve of its surface temperature.As seen from the figure, after 20min, Fiber/P temperature occurs slow
Increase, and stablizes after 60min to~21 DEG C.It follows that when Fiber/P covering high-temperature target, it can be by the way that phase transition damage occurs
A large amount of heat is consumed, the raising of own temperature is slowed down, inhibits the infrared emanation intensity on high-temperature targets surface, is realized good red
Outer stealth effect.
Claims (8)
1. a kind of preparation method of phase transformation Infrared stealthy materials, which is characterized in that method includes the following steps:
(1) collagenous fibres are dispersed with stirring in suitable organic solution uniformly；
(2) it is formed through filtering；
(3) uniform phase-change material is added dropwise；
(4) after drying in the shade naturally, the phase-change material Fiber/P compound with collagenous fibres base can be obtained；
Or,
Naturally after drying in the shade, with organic bond on it top finishing metal powder M reflection layer or its lower surface cover with paint, lacquer, colour wash, etc. aoxidize
Object MOxThe phase-change material Fiber/P/M or MO compound with collagenous fibres base can be obtained in thermal insulation layerx/Fiber/P。
2. preparation method according to claim 1, which is characterized in that the collagenous fibres are with ox-hide, sheepskin or pigskin
For the raw material fiber that routinely method for leather-making produces.
3. preparation method according to claim 1, which is characterized in that the phase-change material is 1 with collagenous fibres mass ratio
~2:1.
4. preparation method according to claim 1, which is characterized in that the phase-change material is paraffin.
5. the preparation method according to claim 4, which is characterized in that the paraffin is 2:1 with collagenous fibres mass ratio.
6. preparation method according to claim 1, which is characterized in that the organic solution is dehydrated alcohol, PDMS solution
Any one in (2wt%, dodecane are solvent), plant polyphenol solution.
7. preparation method according to claim 1, which is characterized in that powder used in the metal powder M reflection coating
For wicker copper (Cu@Ag) or WO3One of (≤5 μm), the organic bond are that (50wt%, dodecane are molten to PDMS
Agent).
8. preparation method according to claim 1, which is characterized in that the oxide M Ox thermal insulation layer is with 100nm
SiO2As heat-insulated oxide, PDMS (50wt%, dodecane are solvent) is used as organic bond.
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Cited By (1)
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| CN115323794A (en) * | 2022-07-07 | 2022-11-11 | 合肥市盛文信息技术有限公司 | Preparation method and application of infrared stealth fabric coating fabric |
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Application publication date: 20181204 |