CN107880854A - A kind of composite phase-change cool storage material and preparation method thereof - Google Patents
A kind of composite phase-change cool storage material and preparation method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
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- C08G18/4829—Polyethers containing at least three hydroxy groups
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
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Abstract
The present invention relates to a kind of composite phase-change cool storage material and preparation method thereof, it belongs to new material technology field.A kind of composite phase-change cool storage material, the material be by organic three-dimensional network gel rubber material by solvent displacement with low-temperature phase-change material is compound is prepared, the mass ratio of described organic three-dimensional network gel rubber material and low-temperature phase-change material is 1：5~10；Wherein, organic three-dimensional network gel rubber material is prepared by polyisocyanates and polyhydric alcohol polymer cross-linked polymeric；The low-temperature phase-change material is water, N, the aqueous solution of N dimethyl sulfoxide (DMSO)s, ethylene glycol or inorganic salts；The mass concentration of the aqueous solution of the inorganic salts is 0.1%~10%.Synthesis technique of the present invention is simple, and using convenient, the material phase transformation enthalpy is big, and cold insulation time length, no liquid leaks during work, can Reusability, have wide application prospects in terms of cold accumulation cooling-down.
Description
Technical field
The present invention relates to a kind of composite phase-change cool storage material and preparation method thereof, it belongs to new material technology field.
Background technology
Phase-changing energy storage material is a kind of by physics phase in version (solid-liquid, liquid-gas etc.) process, absorbs or release is a large amount of
Heat has the advantages of energy storage density is big, and energy storage capacity is strong, can effectively alleviate energy so as to the material realized energy stores Yu utilized
The upper space of amount supply and time are unbalance to conflict, and is one of effective means of raising energy utilization efficiency.
Phase-change material can be divided into phase-change heat-storage material and phase-change material for cold storage according to its application.Phase-change material for cold storage exists
There is great demand in the field such as hot operation temperature control clothes, air-conditioning and cooling system and cold storing and fresh-keeping.
At present, in phase change cold-storage field, using it is more be ice or hydrated salt cold-storage, but this cold-storage mode is present
The problem of very big, the water or hydrated salt of solid-state can produce big quantity of fluid during phase in version, due to convection heat transfer' heat-transfer by convection cold accumulation effects
Rapid drawdown, and liquid caused by thawing may damage electronic device.So the cool storage material with shape stability obtains
The extensive concern of people.
The content of the invention
To solve problems of the prior art, the present invention provides a kind of new composite phase-change cool storage material and its preparation
Method.Composite phase-change cool storage material prepared by the present invention has larger phase transformation enthalpy and suitable phase transition temperature, has excellent
Different cold insulation effect, the leakage of cold insulation process no liquid, and high recycling rate.Such materials synthesis technique is simple, available for reality
Border is applied, and is had broad application prospects.
A kind of composite phase-change cool storage material, the material be by organic three-dimensional network gel rubber material by solvent displacement with
Low-temperature phase-change material is compound to be prepared, and the mass ratio of described organic three-dimensional network gel rubber material and low-temperature phase-change material is 1：
5~10；
Wherein, organic three-dimensional network gel rubber material is prepared into by polyisocyanates and polyhydric alcohol polymer cross-linked polymeric
Arrive；The low-temperature phase-change material is water, N, the aqueous solution of N- dimethyl sulfoxide (DMSO)s, ethylene glycol or inorganic salts；The water of the inorganic salts
The mass concentration of solution is 0.1%~10%, wherein, the inorganic salts are sodium chloride, potassium chloride, sodium sulphate, potassium sulfate, nitric acid
One or more in sodium, potassium nitrate.
Further, the method for the present invention that organic three-dimensional network gel rubber material is compound with low-temperature phase-change material is preferred
For：Organic three-dimensional network gel rubber material containing organic solvent is subjected to solvent displacement under the conditions of ultrasonic wave added with ethanol；After
And solvent displacement occurs with low-temperature phase-change material, and low-temperature phase-change material and organic three-dimensional network gel rubber material is compound, formed multiple
Close cool storage material.
Solvent displacement of the present invention can specifically operate as follows：Organic three-dimensional network gel rubber material is put
Put in enough ethanol, 1~3h of ultrasound, change fresh ethanol and continue ultrasound twice, then the material is placed in enough water,
1~3h of ultrasound, continuation is ultrasonic after changing fresh water, 3 times altogether.
Further, the polyisocyanates be 1B triisocyanate, triphenylmethane triisocyanate, 1,3,
(3- NCOs the tolyl) -1,3,5- triazine -2,4,6- of 5- tri- ketone, toluene di-isocyanate(TDI) and trimethylolpropane addition
Thing, HDI biuret polyisocyanates, tri o cresyl thiophosphate (4- phenyl isocyanates), dimethyl triphenyl methane tetraisocyanate
Deng one kind in polyisocyanates；The polyhydric alcohol polymer is polyethylene glycol, polyvinyl alcohol, polyoxypropyleneglycol, polyoxy
Change one kind in propylene triol, polytetrahydrofuran diol, tetrahydrofuran-propylene oxide copolymer glycols,
Wherein, the mol ratio of the polyisocyanates and polyhydric alcohol polymer is according to hydroxyl in polyhydric alcohol polymer and polyisocyanate
In cyanate-mol ratio of NCO group is 1:1 meter.
Further, described organic solvent is tetrahydrofuran, dioxane, acetone, chloroform, dichloromethane, four chlorinations
1~2 kind in carbon, DMF, DMSO, benzene, toluene, hexamethylene or n-hexane.
The preferably described organic three-dimensional network gel rubber material containing organic solvent of composite phase-change cool storage material of the present invention
It is made as follows：
It is 1 by mass ratio：5~10 polyhydric alcohol polymers mix with organic solvent, 50~100 DEG C of magnetic agitations to polyalcohol
Polymer is completely dissolved；Polyisocyanates is added into above-mentioned resulting solution and dibutyltin dilaurate catalyst, magnetic force stir
0.5~6h is mixed, the cross-linking reaction at 50~100 DEG C, is poured into when solution is sticky in Teflon mold, at 50~100 DEG C
Continue to be crosslinked, form organic three-dimensional network gel rubber material containing organic solvent.
Further, the mass ratio of the dibutyltin dilaurate catalyst and polyhydric alcohol polymer is 1：80~150.
It is a further object of the present invention to provide the preparation method of above-mentioned composite phase-change cool storage material.
A kind of preparation method of composite phase-change cool storage material, comprises the following steps：
(1) it is 1 by mass ratio：5~10 polyhydric alcohol polymers mix with organic solvent, and 50~100 DEG C of magnetic agitations are at most
First alkoxide polymer is completely dissolved；
(2) polyisocyanates and dibutyltin dilaurate catalyst are added in molar ratio into step (1) resulting solution,
0.5~6h of magnetic agitation, the cross-linking reaction at 50~100 DEG C, poured into when solution is sticky in Teflon mold, 50~
Continue to be crosslinked at 100 DEG C, form organic three-dimensional network gel rubber material containing organic solvent；
(3) organic three-dimensional network gel rubber material that this contains organic solvent is carried out under the conditions of ultrasonic wave added with ethanol molten
Agent is replaced, and solvent displacement then occurs with low-temperature phase-change material, low-temperature phase-change material and organic three-dimensional network gel rubber material are answered
Close, form compound cool storage material.
In above-mentioned technical proposal, the organic solvent described in preferred steps (1) is tetrahydrofuran, dioxane, acetone, chlorine
1~2 kind in imitative, dichloromethane, carbon tetrachloride, DMF, DMSO, benzene, toluene, hexamethylene or n-hexane；Step (2) is described to urge
The mass ratio of agent and polyhydric alcohol polymer is 1：80~150.
Beneficial effects of the present invention：The invention provides a kind of new composite phase-change cool storage material, the material phase transformation enthalpy
Value is maximum to have excellent cold insulation between -10~10 DEG C up to 311.4J/g, phase transition temperature between 95~311.4J/g
Effect, the cold insulation time is compared with ice extends 2 times, the liquid phenomenon of leakage will not occur during cold insulation, and circulating frozen thaws and imitated
Fruit is good.The materials synthesis technique is simple, using conveniently, is had broad application prospects in cold accumulation cooling-down field.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of composite phase-change cool storage material in embodiment 1, wherein：A, organic three-dimensional network gel material
Material, b, composite phase-change cool storage material.
Fig. 2 is the DSC curve of composite phase-change cool storage material in embodiment 1.
Fig. 3 be embodiment 1 in gel rubber material and etc. the ice of quality temperature-thawing time curve.
Fig. 4 is temperature-thawing time curve after material involved by embodiment 1 repeatedly freeze-thaw.
Fig. 5 is digital photograph after the pictorial diagram of material involved by embodiment 1 and circulation.
Embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments, it is conventional method unless otherwise specified；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1
(1) it is 1 to take mass ratio:10 polyethylene glycol (Mn=10000) and toluene is heated to gathering in 80 DEG C of waters bath with thermostatic control
Ethylene glycol is completely dissolved；
(2) it is 2 to be added in above-mentioned solution with polyethylene glycol mol ratio:3 triphenylmethane triisocyanate and 3 drops two
Dibutyl tin laurate catalyst, magnetic agitation 6h, the cross-linking reaction at 90 DEG C, Teflon mold is poured into when solution is sticky
In, continue to be crosslinked at 90 DEG C, form organic three-dimensional network gel rubber material containing toluene；
(3) the organic three-dimensional network gel rubber material for containing toluene is placed in enough ethanol, ultrasonic 2h, changed fresh
Ethanol continue ultrasound twice, each 2h；The material is placed in enough water again, ultrasonic 2h, change after fresh water followed by
Continuous ultrasound twice, each 2h, makes water and organic three-dimensional network gel rubber material compound, forms compound cool storage material,
After the above-mentioned phase change cold-storage gel rubber material being prepared is freezed at -12 DEG C and etc. the ice of quality be placed on 25 DEG C
Constant temperature oven in and connect thermocouple record temperature-time curve, test its cold insulation effect, can from curve as a result such as Fig. 3
To see, 0~5 DEG C of low temperature is kept under equal conditions, ice can keep 4155s, and the composite phase-change cool storage material of gained can be with
7800s is kept, cold insulation ability is substantially better than ice.
The above-mentioned phase-change material for cold storage repeated freezing being prepared is thawed 300 times, is placed in 25 DEG C of constant temperature oven
And thermocouple record temperature-time curve is connected, test it and circulate cold insulation, as a result such as Fig. 4, it can be seen that in circulating frozen
After thawing 300 times, the cold insulation time does not have significant change, remains to reach 7800s, illustrates that the material circulation performance is good, service life
It is long.Digital photograph such as Fig. 5 before and after circulation, it can be seen that outward appearance is without significant change before and after material circulation, and because support frame is
The cross-linked polyurethane of three-dimensional network so that the phase-change material for cold storage finally prepared is compared to have compared with conventional hydrogels can preferably add
Work and durability, are not required to additional package, can directly apply.
Fig. 1 is the infrared spectrogram of composite phase-change cool storage material in embodiment 1, wherein：A, organic three-dimensional network gel material
Material, b, composite phase-change cool storage material.1730cm in Fig. 1 a is can be seen that in Fig. 1-1Place belongs to C=O stretching vibration peak,
1359、1240cm-1Locate the symmetrically and asymmetrically stretching vibration peak for C-N, the appearance at these peaks proves isocyanates and poly- second
The condensation reaction of glycol.3277 and 1635cm in Fig. 1 b-1Place is the characteristic peak of water, and the infrared spectrum is almost organic three-dimensional solidifying
Glue material is superimposed with the infrared spectrum of water, is occurred without new peak, is illustrated that between organic three dimensional gel material and water be physics
Compound, chemical reaction does not occur.But the peak intensity of organic three dimensional gel material significantly declines, this is due to compound
The content of material reclaimed water is very high, so the feature peak intensity of infrared spectrum reclaimed water is larger, and polyethers in organic three dimensional gel material
Content is larger, so polyethers peak (1092cm in composite spectrum-1) intensity is larger.The DSC of gained phase change cold-storage gel rubber material
Curve, such as Fig. 2.Visible in Fig. 2, the phase transformation enthalpy of the material of gained reaches 311.4J/g, close to the phase transformation enthalpy (335J/ of ice
G), this is due to that substantial amounts of ice present in composite destroys Polyethylene glycol crystal after freezing, and the interconvertibility of ice is only presented
Energy.
Embodiment 2-4
The mass ratio of polyethylene glycol (Mn=10000) and toluene is changed to 1 respectively:5,1:7,1:9, obtain corresponding phase transformation
Cold-storage gel rubber material, other conditions are consistent with embodiment 1.Measurement result shows, the phase change cold-storage gel rubber material phase being prepared
Become enthalpy and reach 250J/g.
Embodiment 5-6
By N, N- dimethyl sulfoxide (DMSO)s, ethylene glycol obtain corresponding phase change cold-storage gel rubber material as low-temperature phase-change material, its
His condition is consistent with embodiment 1.
Embodiment 7-8
Using the sodium-chloride water solution of mass concentration 3% and 5% potassium chloride solution as low-temperature phase-change material, phase is obtained
The phase change cold-storage gel rubber material answered, other conditions are consistent with embodiment 1.
Embodiment 9-16
Using tetrahydrofuran, dioxane, acetone, chloroform, dichloromethane, carbon tetrachloride, DMF, DMSO as crosslinking
The solvent of reaction, obtains corresponding phase change cold-storage gel rubber material, and other conditions are consistent with embodiment 1.
Embodiment 17-20
Polyethylene glycol is changed to polyoxypropyleneglycol, PPOX triol, polytetrahydrofuran diol, tetrahydrochysene furan respectively
Mutter-propylene oxide copolymer glycols, obtain corresponding phase change cold-storage gel rubber material, other conditions are consistent with embodiment 1.
Embodiment 21-23
1 is changed to respectively using polyoxypropyleneglycol as polymeric component, and the mass ratio of toluene:5,1:7,1:9, obtain phase
The phase change cold-storage gel rubber material answered, other conditions are consistent with embodiment 17.
Embodiment 24-27
By crosslinking agent triphenylmethane triisocyanate is changed to 1B triisocyanate respectively, (3- is different by 1,3,5- tri-
Cyanic acid ester group tolyl) -1,3,5- triazine -2,4,6- ketone, toluene di-isocyanate(TDI) and trimethylolpropane addition product, HDI contracting
Two urea polyisocyanates, obtain corresponding phase change cold-storage gel rubber material, and other conditions are consistent with embodiment 1.
Embodiment 28-32
It is water-soluble with 3% potassium chloride solution, 3% aqueous sodium persulfate solution, 3% potassium sulfate solution, 3% sodium nitrate respectively
Liquid, 3% Alkitrate obtain corresponding phase change cold-storage gel rubber material, other conditions are with implementing as low-temperature phase-change material
Example 7 is consistent.
Claims (7)
- A kind of 1. composite phase-change cool storage material, it is characterised in that：The material be passed through by organic three-dimensional network gel rubber material it is molten Agent displacement method with low-temperature phase-change material is compound is prepared, described organic three-dimensional network gel rubber material and low-temperature phase-change material Mass ratio is 1：5~10；Wherein, organic three-dimensional network gel rubber material is prepared by polyisocyanates and polyhydric alcohol polymer cross-linked polymeric；Institute Low-temperature phase-change material is stated as water, N, the aqueous solution of N- dimethyl sulfoxide (DMSO)s, ethylene glycol or inorganic salts；The aqueous solution of the inorganic salts Mass concentration is 0.1%~10%, wherein, the inorganic salts are sodium chloride, potassium chloride, sodium sulphate, potassium sulfate, sodium nitrate, nitre One or more in sour potassium.
- 2. material according to claim 1, it is characterised in that：It is described by organic three-dimensional network gel rubber material and low temperature phase change The method of Material cladding is：Organic three-dimensional network gel rubber material containing organic solvent is entered under the conditions of ultrasonic wave added with ethanol Row solvent is replaced；Then solvent displacement occurs with low-temperature phase-change material, by low-temperature phase-change material and organic three-dimensional network gel material Expect compound, form compound cool storage material.
- 3. material according to claim 1, it is characterised in that：The polyisocyanates be 1B triisocyanate, Triphenylmethane triisocyanate, (3- NCOs the tolyl) -1,3,5- triazine -2,4,6- of 1,3,5- tri- ketone, toluene two Isocyanates and trimethylolpropane addition product, HDI biuret polyisocyanates, tri o cresyl thiophosphate (4- phenyl isocyanates), One kind in the polyisocyanates such as dimethyl triphenyl methane tetraisocyanate；The polyhydric alcohol polymer is polyethylene glycol, gathered Vinyl alcohol, polyoxypropyleneglycol, PPOX triol, polytetrahydrofuran diol, tetrahydrofuran-propylene oxide copolymer glycols In one kind,Wherein, the mol ratio of the polyisocyanates and polyhydric alcohol polymer is according to hydroxyl in polyhydric alcohol polymer and polyisocyanic acid In ester-mol ratio of NCO group is 1:1 meter.
- 4. material according to claim 2, it is characterised in that：Described organic solvent is tetrahydrofuran, dioxane, third 1~2 kind in ketone, chloroform, dichloromethane, carbon tetrachloride, DMF, DMSO, benzene, toluene, hexamethylene or n-hexane.
- 5. according to the material described in any one of claim 2~4, it is characterised in that：Organic three-dimensional containing organic solvent Network gel material is made as follows：It is 1 by mass ratio：5~10 polyhydric alcohol polymers mix with organic solvent, 50~ 100 DEG C of magnetic agitation to polyhydric alcohol polymers are completely dissolved；Polyisocyanates and tin dilaurate are added into above-mentioned resulting solution Dibutyl tin catalyst, 0.5~6h of magnetic agitation, the cross-linking reaction at 50~100 DEG C, tetrafluoroethene is poured into when solution is sticky In mould, continue to be crosslinked at 50~100 DEG C, form organic three-dimensional network gel rubber material containing organic solvent.
- 6. material according to claim 5, it is characterised in that：The dibutyltin dilaurate catalyst gathers with polyalcohol The mass ratio of compound is 1：80~150.
- 7. the preparation method of the composite phase-change cool storage material described in any one of claim 1~6, it is characterised in that：Including with Lower step：(1) it is 1 by mass ratio：5~10 polyhydric alcohol polymers mix with organic solvent, 50~100 DEG C of magnetic agitations to polyalcohol Polymer is completely dissolved；(2) polyisocyanates and dibutyltin dilaurate catalyst, magnetic force are added in molar ratio into step (1) resulting solution 0.5~6h is stirred, the cross-linking reaction at 50~100 DEG C, is poured into when solution is sticky in Teflon mold, at 50~100 DEG C Under continue to be crosslinked, form organic three-dimensional network gel rubber material containing organic solvent；(3) organic three-dimensional network gel rubber material that this contains organic solvent is carried out into solvent with ethanol under the conditions of ultrasonic wave added to put Change, solvent displacement, low-temperature phase-change material and organic three-dimensional network gel rubber material is compound, shape then occur with low-temperature phase-change material Into compound cool storage material.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110846721A (en) * | 2019-10-12 | 2020-02-28 | 湖南理工学院 | Monocrystalline silicon texturing additive formula containing polyalcohol and PEG |
| WO2020077554A1 (en) * | 2018-10-17 | 2020-04-23 | Dow Global Technologies Llc | Gel comprising phase change materials |
| CN111808577A (en) * | 2020-05-27 | 2020-10-23 | 纯钧新材料(深圳)有限公司 | High-stability composite phase-change gel for cold chain transportation of 2-8 ℃ medicines |
| CN111826131A (en) * | 2020-05-27 | 2020-10-27 | 纯钧新材料(深圳)有限公司 | Preparation method of high-stability composite phase-change gel for cold chain transportation of 2-8 ℃ medicines |
| CN111961228A (en) * | 2020-08-24 | 2020-11-20 | 中冶武汉冶金建筑研究院有限公司 | Composite phase-change cold storage material hydrogel and preparation method and application thereof |
| CN113527573A (en) * | 2021-07-23 | 2021-10-22 | 苏州双碳新材料有限公司 | Preparation method of phase-change gel material with variable mechanical state |
| CN113583635A (en) * | 2021-07-23 | 2021-11-02 | 苏州双碳新材料有限公司 | Phase-change gel material with variable mechanical state |
| CN115368875A (en) * | 2022-08-31 | 2022-11-22 | 苏州大学 | Flexible ice-based cold accumulation composite material and preparation method thereof |
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| CN111826131A (en) * | 2020-05-27 | 2020-10-27 | 纯钧新材料(深圳)有限公司 | Preparation method of high-stability composite phase-change gel for cold chain transportation of 2-8 ℃ medicines |
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| CN115368875A (en) * | 2022-08-31 | 2022-11-22 | 苏州大学 | Flexible ice-based cold accumulation composite material and preparation method thereof |
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