CN107880854B - 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
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having 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
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Abstract
The present invention relates to a kind of composite phase-change cool storage materials and preparation method thereof, belong 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 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, ethylene glycol or inorganic salts；The mass concentration of the aqueous solution of the inorganic salts is 0.1%~10%.Synthesis technology of the present invention is simple, and using convenient, the material phase transformation enthalpy is big, and the cold insulation time is long, and 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 materials and preparation method thereof, belong to new material technology field.
Background technique
Phase-changing energy storage material is a kind of by physics phase transition (solid-liquid, liquid-gas etc.) process, absorbs or release is a large amount of
Material of the heat to realize energy stores with utilize, has energy storage density big, energy can be effectively relieved in the strong advantage of energy storage capacity
Amount supply upper space and time it is unbalance conflict, be one of the 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 range.Phase-change material for cold storage exists
There is great demand in hot operation temperature control clothes, air-conditioning and the fields such as cooling system and cold storing and fresh-keeping.
Currently, in phase change cold-storage field, using it is more be ice or hydrated salt cold-storage, but this cold-storage mode exists
Very big problem, solid water or hydrated salt can generate big quantity of fluid during phase transition, due to convective heat transfer cold accumulation effects
Rapid drawdown, and melt the liquid generated and may be damaged electronic device.So the cool storage material with shape stability obtains
The extensive concern of people.
Summary of the invention
To solve problems of the prior art, the present invention provides a new class of composite phase-change cool storage material and its preparation
Method.Composite phase-change cool storage material prepared by the present invention has biggish 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 simple process, can be used for reality
Border application, has 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 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
It arrives；The low-temperature phase-change material is water, N, the aqueous solution of N- dimethyl sulfoxide, 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 of sodium, potassium nitrate are a variety of.
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
Are as follows: organic three-dimensional network gel rubber material containing organic solvent is subjected to solvent displacement with ethyl alcohol under the conditions of ultrasonic wave added；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, it is 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
It sets in enough ethyl alcohol, 1~3h of ultrasound, replaces fresh ethyl alcohol and continue ultrasound twice, then the material is placed in enough water,
1~3h of ultrasound continues ultrasound after replacing fresh water, amounts to 3 times.
Further, the polyisocyanates be L-lysine triisocyanate, triphenylmethane triisocyanate, 1,3,
(3- isocyanate group the tolyl) -1,3,5- triazine -2,4,6- of 5- tri- ketone, toluene di-isocyanate(TDI) and trimethylolpropane addition
Object, HDI biuret polyisocyanate, tri o cresyl thiophosphate (4- phenyl isocyanate), dimethyl triphenyl methane tetraisocyanate
One of equal polyisocyanates；The polyhydric alcohol polymer is polyethylene glycol, polyvinyl alcohol, polyoxypropyleneglycol, polyoxy
Change one of propylene triol, polytetrahydrofuran diol, tetrahydrofuran-propylene oxide copolymer glycols,
Wherein, the molar ratio of the polyisocyanates and polyhydric alcohol polymer is according to hydroxyl and polyisocyanate in polyhydric alcohol polymer
In cyanate-molar ratio of NCO group is 1:1 meter.
Further, the organic solvent is tetrahydrofuran, dioxane, acetone, chloroform, methylene chloride, 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:
Mass ratio is mixed for the polyhydric alcohol polymer of 1:5~10 with organic solvent, 50~100 DEG C of magnetic agitations to polyalcohol
Polymer is completely dissolved；Polyisocyanates is added into above-mentioned acquired 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 Teflon mold when solution is sticky, at 50~100 DEG C
Continue to be crosslinked, forms 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 methods of above-mentioned composite phase-change cool storage material.
A kind of preparation method of composite phase-change cool storage material, comprising the following steps:
(1) mass ratio is mixed for the polyhydric alcohol polymer of 1:5~10 with organic solvent, 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) acquired solution,
0.5~6h of magnetic agitation, the cross-linking reaction at 50~100 DEG C, is poured into Teflon mold when solution is sticky, 50~
Continue to be crosslinked at 100 DEG C, forms organic three-dimensional network gel rubber material containing organic solvent；
(3) the organic three-dimensional network gel rubber material for containing organic solvent is carried out under the conditions of ultrasonic wave added with ethyl alcohol molten
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 for agent displacement
It closes, forms compound cool storage material.
In above-mentioned technical proposal, organic solvent described in preferred steps (1) is tetrahydrofuran, dioxane, acetone, chlorine
1~2 kind in imitative, methylene chloride, 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 present invention provides a kind of novel composite phase-change cool storage material, the material phase transformation enthalpys
Value is maximum up to 311.4J/g between 95~311.4J/g, and phase transition temperature has excellent cold insulation between -10~10 DEG C
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 imitates
Fruit is good.The materials synthesis simple process has broad application prospects using conveniently in cold accumulation cooling-down field.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of composite phase-change cool storage material in embodiment 1, in which: 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 and circulation of material involved by embodiment 1.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1
(1) mass ratio is taken to be heated to gathering in 80 DEG C of waters bath with thermostatic control for the polyethylene glycol (Mn=10000) and toluene of 1:10
Ethylene glycol is completely dissolved；
(2) it is added in the above solution and the triphenylmethane triisocyanate that polyethylene glycol molar ratio is 2:3 and 3 drops two
Dibutyl tin laurate catalyst, magnetic agitation 6h, the cross-linking reaction at 90 DEG C pour into Teflon mold when solution is sticky
In, continue to be crosslinked at 90 DEG C, forms organic three-dimensional network gel rubber material containing toluene；
(3) organic three-dimensional network gel rubber material containing toluene is placed in enough ethyl alcohol, ultrasonic 2h, is replaced fresh
Ethyl alcohol continue ultrasound twice, each 2h；The material is placed in enough water again, ultrasonic 2h, replace after fresh water followed by
Twice, each 2h keeps water and organic three-dimensional network gel rubber material compound, forms compound cool storage material continuous ultrasound,
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 resulting composite phase-change cool storage material 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, it tests it and recycles 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.Circulation front and back digital photograph such as Fig. 5, it can be seen that appearance is without significant change before and after material circulation, and since support frame is
The cross-linked polyurethane of three-dimensional network, so that the phase-change material for cold storage finally prepared is compared compared with conventional hydrogels to be had preferably and can 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, in which: a, organic three-dimensional network gel material
Material, b, composite phase-change cool storage material.It can be seen that 1730cm in Fig. 1 a in Fig. 1-1Place belongs to the stretching vibration peak of C=O,
1359、1240cm-1Place is the symmetrically and asymmetrically stretching vibration peak of C-N, and 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, which is almost organic three-dimensional solidifying
Glue material is superimposed with the infrared spectrum of water, and not new peak occurs, and illustrates that between organic three dimensional gel material and water be physics
Compound, there is no chemical reactions to occur.But the equal sharp fall of peak intensity of organic three dimensional gel material, this is because compound
The content of water is very high in material, so the feature peak intensity of water is larger in infrared spectroscopy, and polyethers in organic three dimensional gel material
Content is larger, so polyethers peak (1092cm in composite material spectrum-1) intensity is larger.The DSC of gained phase change cold-storage gel rubber material
Curve, such as Fig. 2.As it can be seen that the phase transformation enthalpy of resulting material reaches 311.4J/g in Fig. 2, close to the phase transformation enthalpy (335J/ of ice
G), this is because a large amount of ice present in composite material destroys Polyethylene glycol crystal after freezing, the interconvertibility of ice is only presented
Energy.
Embodiment 2-4
The mass ratio of polyethylene glycol (Mn=10000) and toluene is changed to 1:5,1:7,1:9 respectively, obtains corresponding phase transformation
Cold-storage gel rubber material, other conditions and embodiment 1 are consistent.Measurement result shows, the phase change cold-storage gel rubber material phase being prepared
Become enthalpy and reaches 250J/g.
Embodiment 5-6
By N, N- dimethyl sulfoxide, ethylene glycol obtain corresponding phase change cold-storage gel rubber material as low-temperature phase-change material,
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, obtain phase
The phase change cold-storage gel rubber material answered, other conditions and embodiment 1 are consistent.
Embodiment 9-16
Using tetrahydrofuran, dioxane, acetone, chloroform, methylene chloride, carbon tetrachloride, DMF, DMSO as crosslinking
The solvent of reaction, obtains corresponding phase change cold-storage gel rubber material, and other conditions and embodiment 1 are consistent.
Embodiment 17-20
Polyethylene glycol is changed to polyoxypropyleneglycol, polypropylene oxide triol, polytetrahydrofuran diol, tetrahydro furan respectively
It mutters-propylene oxide copolymer glycols, obtains corresponding phase change cold-storage gel rubber material, other conditions and embodiment 1 are consistent.
Embodiment 21-23
It is changed to 1:5,1:7,1:9 respectively using polyoxypropyleneglycol as the mass ratio of polymeric component and toluene, obtains phase
The phase change cold-storage gel rubber material answered, other conditions and embodiment 17 are consistent.
Embodiment 24-27
Crosslinking agent triphenylmethane triisocyanate is changed to L-lysine triisocyanate, (3- is different by 1,3,5- tri- respectively
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 and embodiment 1 are consistent.
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% potassium nitrate aqueous solution obtain corresponding phase change cold-storage gel rubber material, other conditions and implementation as low-temperature phase-change material
Example 7 is consistent.
Claims (7)
1. a kind of composite phase-change cool storage material, it is characterised in that: the material is by organic three-dimensional network gel rubber material by molten
Agent displacement method with low-temperature phase-change material is compound is prepared, 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
Stating low-temperature phase-change material is water, N, the aqueous solution of N- dimethyl sulfoxide, 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, potassium nitrate
One of or it is a variety of.
2. material according to claim 1, it is characterised in that: described by organic three-dimensional network gel rubber material and low temperature phase change
The method of Material cladding are as follows: by organic three-dimensional network gel rubber material containing organic solvent under the conditions of ultrasonic wave added with ethyl alcohol into
The displacement of row solvent；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, forms compound cool storage material.
3. material according to claim 1, it is characterised in that: the polyisocyanates be L-lysine triisocyanate,
Triphenylmethane triisocyanate, (3- isocyanate group the tolyl) -1,3,5- triazine -2,4,6- of 1,3,5- tri- ketone, toluene two
Isocyanates and trimethylolpropane addition product, HDI biuret polyisocyanate, tri o cresyl thiophosphate (4- phenyl isocyanate),
One of dimethyl triphenyl methane tetraisocyanate；The polyhydric alcohol polymer is polyethylene glycol, polyvinyl alcohol, polyoxygenated
One of propylene glycol, polypropylene oxide triol, polytetrahydrofuran diol, tetrahydrofuran-propylene oxide copolymer glycols,
Wherein, the molar ratio of the polyisocyanates and polyhydric alcohol polymer is according to hydroxyl and polyisocyanic acid in polyhydric alcohol polymer
In ester-molar ratio of NCO group is 1:1 meter.
4. material according to claim 2, it is characterised in that: the organic solvent is tetrahydrofuran, dioxane, third
1 ~ 2 kind in ketone, chloroform, methylene chloride, carbon tetrachloride, DMF, DMSO, benzene, toluene, hexamethylene or n-hexane.
5. according to the described in any item materials of claim 2 ~ 4, it is characterised in that: organic three dimensional network containing organic solvent
Network gel rubber material is made as follows: mass ratio being mixed for the polyhydric alcohol polymer of 1:5 ~ 10 with organic solvent, 50 ~ 100 DEG C
Magnetic agitation to polyhydric alcohol polymer is completely dissolved；Polyisocyanates and di lauric dibutyl are added into above-mentioned acquired solution
Tin catalyst, 0.5 ~ 6 h of magnetic agitation, the cross-linking reaction at 50 ~ 100 DEG C are poured into Teflon mold when solution is sticky,
Continue to be crosslinked at 50 ~ 100 DEG C, forms 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 and polyalcohol are poly-
The mass ratio for closing object is 1:80 ~ 150.
7. the preparation method of composite phase-change cool storage material described in claim 5, it is characterised in that: the following steps are included:
(1) mass ratio is mixed for the polyhydric alcohol polymer of 1:5 ~ 10 with organic solvent, 50 ~ 100 DEG C of magnetic agitations are poly- to polyalcohol
Object is closed to be completely dissolved；
(2) addition polyisocyanates and dibutyltin dilaurate catalyst into step (1) acquired solution, magnetic agitation 0.5 ~
6 h, the cross-linking reaction at 50 ~ 100 DEG C, are poured into Teflon mold when solution is sticky, continue to be crosslinked at 50 ~ 100 DEG C,
Form organic three-dimensional network gel rubber material containing organic solvent；
(3) the organic three-dimensional network gel rubber material for containing organic solvent solvent is carried out with ethyl alcohol under the conditions of ultrasonic wave added to set
It changes, solvent displacement, low-temperature phase-change material and organic three-dimensional network gel rubber material is compound, shape then occurs with low-temperature phase-change material
At compound cool storage material.
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| WO2020077554A1 (en) * | 2018-10-17 | 2020-04-23 | Dow Global Technologies Llc | Gel comprising phase change materials |
| CN110846721A (en) * | 2019-10-12 | 2020-02-28 | 湖南理工学院 | Monocrystalline silicon texturing additive formula containing polyalcohol and PEG |
| CN111826131B (en) * | 2020-05-27 | 2021-07-23 | 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 |
| 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 |
| 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 |
| CN113527573B (en) * | 2021-07-23 | 2023-01-24 | 苏州双碳新材料有限公司 | Preparation method of phase-change gel material with variable mechanical state |
| CN113583635B (en) * | 2021-07-23 | 2023-01-24 | 苏州双碳新材料有限公司 | Phase-change gel material with variable mechanical state |
| CN115368875B (en) * | 2022-08-31 | 2023-07-25 | 苏州大学 | Flexible ice-based cold accumulation composite material and preparation method thereof |
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