CN114686017B - Phase-change energy-storage heat-conducting material and preparation process thereof - Google Patents
Phase-change energy-storage heat-conducting material and preparation process thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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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
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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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- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/14—Thermal energy storage
Abstract
The invention discloses a phase-change energy-storage heat-conducting material and a preparation process thereof, wherein the phase-change energy-storage heat-conducting material comprises the following raw material components in parts by weight: 8-32 parts of liquid silicon rubber, 2-10 parts of zeolite molecular sieve, 30-50 parts of phase-change paraffin and 20-30 parts of spherical boron nitride; wherein the phase change paraffin comprises a thermoplastic resin containing vinyl and a thermoplastic hydrogenated resin. The phase-change energy-storage heat-conducting material has the advantages of certain toughness, mechanical strength and strong stability.
Description
Technical Field
The invention relates to the field of heat conducting materials, in particular to a phase-change energy-storage heat conducting material and a preparation process thereof.
Background
The traditional phase-change energy storage material takes paraffin as a main material, takes phase-change paraffin as an example at a phase-change temperature, and can have the following problems: when the temperature of the product is lower than the phase change point, the toughness and mechanical strength of the product are poor; after the temperature of the product is higher than the phase change point, the product melts and flows, and if the heat conducting filler such as aluminum oxide, aluminum hydroxide, aluminum nitride, boron nitride and the like is added in the system, the paraffin can be separated from the filler, and the paraffin cannot be recovered after the temperature is reduced, so that the material is invalid.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention aims to provide a phase-change energy-storage heat-conducting material and a preparation process thereof, which have good stability, and the product does not flow and deform when the temperature is repeatedly increased and decreased above and below the phase-change point.
In order to achieve the above purpose, the embodiment of the invention provides a phase-change energy-storage heat-conducting material, which comprises the following raw material components in parts by weight: 8-32 parts of liquid silicon rubber, 2-10 parts of zeolite molecular sieve, 30-35 parts of phase-change paraffin and 20-30 parts of spherical boron nitride; wherein the phase change paraffin comprises a thermoplastic resin containing vinyl and a thermoplastic hydrogenated resin.
In one or more embodiments of the present invention, the phase change paraffin comprises 10% to 90% of a vinyl-containing thermoplastic resin and 90% to 10% of a thermoplastic hydrogenated resin in weight fractions.
In one or more embodiments of the invention, the zeolite molecular sieve is a 250-350 mesh particle.
In one or more embodiments of the invention, the spherical boron nitride is graded spherical boron nitride.
The embodiment of the invention also provides a preparation process of the phase-change energy-storage heat-conducting material, which comprises the following steps: according to the weight portion, 8 to 32 portions of liquid silicon rubber, 2 to 10 portions of zeolite molecular sieve, 30 to 35 portions of phase-change paraffin and 20 to 30 portions of spherical boron nitride are evenly mixed to obtain an intermediate product; and adding a catalyst into the intermediate product, reacting to obtain a pre-product, and cooling the pre-product to obtain the phase-change energy storage heat-conducting material.
In one or more embodiments of the present invention, the liquid silicone rubber, zeolite molecular sieve, phase change paraffin, and spherical boron nitride are stirred uniformly at a temperature of 55 to 65 ℃ to obtain an intermediate product.
In one or more embodiments of the invention, the catalyst is a platinum catalyst.
In one or more embodiments of the invention, the mass ratio of the catalyst to the intermediate is (0.01 to 0.2): 100.
in one or more embodiments of the invention, the reaction conditions are: the temperature is 130-140 ℃ and the time is 0.5-3h.
In one or more embodiments of the invention, the cooling of the pre-product is specifically cooling the pre-product to room temperature.
Compared with the prior art, according to the phase-change energy-storage heat-conducting material and the preparation process thereof, the thermoplastic resin containing vinyl and the hydrogen-containing silicone oil in the liquid silicone rubber are subjected to crosslinking reaction at 130 ℃ to generate part of organic silicone wax. The organosilicon wax and paraffin which does not participate in the reaction form a gel structure, and the phase change can occur at a temperature higher than the phase change, but has extremely high viscosity and does not flow. At the temperature lower than the phase transition temperature, the porous liquid silicone rubber is used as a strength support, has certain elasticity and stiffness, and the phase transition paraffin between the pores is adsorbed and locked by the molecular sieve and cannot flow freely. So that the phase-change energy-storage heat-conducting material has certain toughness and mechanical strength when the phase-change temperature is lower than the phase-change temperature of the phase-change energy-storage heat-conducting material; or the phase-change energy-storage heat-conducting material has stronger stability when the phase-change temperature is higher than the phase-change temperature of the phase-change energy-storage heat-conducting material, so that the possibility of separating each component of the phase-change energy-storage heat-conducting material is reduced.
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
The phase-change energy-storage heat-conducting material according to the preferred embodiment of the invention comprises the following raw material components in parts by weight: 8-32 parts of liquid silicon rubber, 2-10 parts of zeolite molecular sieve, 30-35 parts of phase-change paraffin and 20-30 parts of spherical boron nitride; wherein the phase change paraffin comprises a thermoplastic resin containing vinyl and a thermoplastic hydrogenated resin.
The thermoplastic resin containing vinyl can be subjected to crosslinking reaction with hydrogen-containing silicone oil in liquid silicone rubber at 130 ℃ under the action of a catalyst to generate partial organic silicone wax, the organic silicone wax and paraffin which does not participate in the reaction form a gel structure, and the thermoplastic resin can undergo phase change at high temperature (which can be understood as being higher than the phase change temperature of the phase change energy storage heat conduction material), but has extremely high viscosity and does not flow. Therefore, the phase-change energy-storage heat-conducting material still has good stability at high temperature, and can not be recovered after cooling.
Wherein each part may represent 1g, 2g, 10g, 1kg, etc., the mass represented by each part is adjusted according to the mass of the phase change energy storage thermally conductive material being produced.
The phase change paraffin wax may include 40-60% of a thermoplastic resin containing vinyl groups and 60-40% of a thermoplastic hydrogenated resin in weight fraction. thevinyl-containingthermoplasticresinmaybespecificallyPCM-A-44HofGuangzhouNewmaterialstechnologyCo.,Ltd; the thermoplastic hydrogenated resin may specifically be R1090 of Izeman.
The zeolite molecular sieve may be 250-350 mesh particles. The liquid silicone rubber can be RH-G7-1011 of Zhejiang Rumex organosilicon. The spherical boron nitride can be GBN-60 of hundred-picture high-new material technology.
The product has porous liquid silicon rubber as strength support at high temperature, has certain elasticity and stiffness, and phase-change paraffin between pores is adsorbed and locked by zeolite molecular sieve and cannot flow freely; the product can keep the cut shape unchanged in the repeated heating and cooling processes.
Wherein, the spherical boron nitride can be graded spherical boron nitride. In particular to a secondary grading system formed by spherical boron nitride with two different particle sizes. The D50 particle sizes of the two spherical boron nitrides in the secondary grading system are respectively 115-125 mu m of D50 of spherical boron nitride I and 55-65 mu m of D50 of spherical boron nitride II based on the diameter of the spherical boron nitride, and the spherical boron nitride II in the secondary grading system accounts for 10-30% of the total mass of the spherical boron nitride.
The spherical boron nitride of the secondary grading system improves the combination and heat conduction of the spherical boron nitride, liquid silicone rubber, zeolite molecular sieve and phase-change paraffin in the system, reduces the possible void ratio caused by the mixing reaction of the components in the material, thereby reducing the heat transfer obstruction of the phase-change paraffin and improving the effect and the effect of the phase-change paraffin as a heat conducting material in heat transfer. Thereby having remarkable improvement in the aspect of overall heat conducting performance.
The preparation process of the phase-change energy-storage heat-conducting material can comprise the following steps:
and uniformly mixing the liquid silicon rubber, the zeolite molecular sieve, the phase-change paraffin and the spherical boron nitride to obtain an intermediate product.
The steps can be specifically as follows: liquid silicon rubber, zeolite molecular sieve, phase-change paraffin and spherical boron nitride are stirred uniformly at the temperature of 55-65 ℃ to obtain an intermediate product.
And adding a catalyst into the intermediate product, reacting to obtain a pre-product, and cooling the pre-product to obtain the phase-change energy storage heat-conducting material.
Wherein the catalyst may be a platinum catalyst. The platinum catalyst can be specifically 3000ppm of PC12 in Shanghai neutron star chemical industry. The mass ratio of the catalyst to the intermediate product is (0.01-0.2): 100. the reaction conditions may specifically be: the temperature is 130-140 ℃ and the reaction time is 0.5-3h.
The step of cooling the pre-product is specifically to cool the pre-product to room temperature.
In order to facilitate preparation and forming, the raw materials can be added into a corresponding mold to perform the reaction, and after the reaction is finished, the phase-change energy storage heat-conducting material with a corresponding shape can be obtained by cooling. Such as flakes, blocks, spheres, etc.
In the case of example 1,
80GofRH-G7-1011,30Gofzeolitemolecularsieve,150GofPCM-A-44H,150GofR1090,40GofGBN-60withD50=60mumand160GofGBN-60withD50=115mumareuniformlystirredat55℃,then0.5GofPC12isadded,thetemperatureisraisedto130℃afteruniformmixing,thenPETreleasefilmiscoatedonbothsidesafterreactionfor1h,a200x2.0mmsampleispreparedbyhotrolling,andthephasechangeenergystorageheatconductionmaterialisobtainedaftercoolingtoroomtemperature.
In the case of example 2,
120GofRH-G7-1011,25Gofzeolitemolecularsieve,120GofPCM-A-44H,180GofR1090,40GofGBN-60withD50=65mumand160GofGBN-60withD50=125mumareuniformlystirredat55℃,then0.5GofPC12isadded,thetemperatureisraisedto130℃afteruniformmixing,thenPETreleasefilmiscoatedonbothsidesafterreactionfor1h,a200x2.0mmsampleispreparedbyhotrolling,andthephasechangeenergystorageheatconductionmaterialisobtainedaftercoolingtoroomtemperature.
In the case of example 3,
100GofRH-G7-1011,40Gofzeolitemolecularsieve,180GofPCM-A-44H,120GofR1090,40GofGBN-60withD50=55mumand160GofGBN-60withD50=120mumareuniformlystirredat55℃,then0.5GofPC12isadded,afteruniformmixing,thetemperatureisraisedto140℃,after2hoursofreaction,PETreleasefilmiscoatedonbothsides,a200x2.0mmsampleispreparedbyhotrolling,andthephasechangeenergystorageheatconductionmaterialisobtainedaftercoolingtoroomtemperature.
In the case of example 4,
80GofRH-G7-1011,25Gofzeolitemolecularsieve,150GofPCM-A-44H,150GofR1090,60GofGBN-60withD50=60mumand180GofGBN-60withD50=115mumareuniformlystirredat65℃,then1.3GofPC12isadded,afteruniformmixing,thetemperatureisraisedto135℃,after3hoursofreaction,PETreleasefilmiscoatedonbothsides,a200x2.0mmsampleispreparedbyhotrolling,andthephasechangeenergystorageheatconductionmaterialisobtainedaftercoolingtoroomtemperature.
In example 5 the process was carried out,
320GofRH-G7-1011,20Gofzeolitemolecularsieve,175GofPCM-A-44H,175GofR1090,26GofGBN-60withD50=60mumand260GofGBN-60withD50=115mumareuniformlystirredat60℃,then0.1GofPC12isadded,afteruniformmixing,thetemperatureisraisedto130℃,after0.5hofreaction,PETreleasefilmiscoatedonbothsides,a200x2.0mmsampleispreparedbyhotrolling,andthephasechangeenergystorageheatconductionmaterialisobtainedaftercoolingtoroomtemperature.
In example 6 the process was carried out,
160GofRH-G7-1011,100Gofzeolitemolecularsieve,160GofPCM-A-44H,160GofR1090,40GofGBN-60withD50=60mumand260GofGBN-60withD50=115mumareuniformlystirredat55℃,then0.5GofPC12isadded,thetemperatureisraisedto130℃afteruniformmixing,thenPETreleasefilmiscoatedonbothsidesafterreactionfor1h,a200x2.0mmsampleispreparedbyhotrolling,andthephasechangeenergystorageheatconductionmaterialisobtainedaftercoolingtoroomtemperature.
Comparative example 1
25gofzeolitemolecularsieve,150gofPCM-A-44H,150gofR1090,40gofGBN-60withD50=15mumand160gofGBN-60withD50=115mumareuniformlystirredat55℃,then0.5gofPC12isadded,afteruniformmixing,thetemperatureisraisedto130℃,after1hofreaction,PETreleasefilmiscoatedonthetwosides,a200.200.0mmsampleispreparedbyhotrolling,andthephasechangeenergystorageheatconductionmaterialisobtainedaftercoolingtoroomtemperature.
The phase-change energy-storage heat-conducting materials prepared in examples 1 to 6 and the phase-change energy-storage heat-conducting material prepared in comparative example 1 were subjected to performance tests of heat conductivity, phase-change enthalpy and viscosity at 80 ℃):
| coefficient of thermal conductivity (W/m.times.k) | Enthalpy value of phase transition (J/g) | Viscosity at 80 ℃ (cp) | |
| Example 1 | 1.13 | 58.7 | 520000 |
| Example 2 | 1.15 | 48.2 | 570000 |
| Example 3 | 1.12 | 71.4 | 460000 |
| Example 4 | 0.78 | 71.1 | 270000 |
| Example 5 | 0.77 | 71.2 | 220000 |
| Example 6 | 0.77 | 33.4 | 360000 |
| Comparative example 1 | 1.32 | 68.7 | 2300 |
From the viscosity data at 80 ℃ of examples 1, 2, 3, 4, 5, 6 and comparative example 1 in the above table, it can be known that the phase-change energy-storage heat-conducting material of the present invention has high viscosity at high temperature, and the viscosity can maintain a certain high temperature stability, and flow or dislocation cannot easily occur.
From other data in the table above, it can be known that the phase-change energy-storage heat-conducting material of the present invention also has a higher thermal conductivity and a higher phase-change enthalpy value.
Compared with the conventional phase change energy storage material, the product has high viscosity at high temperature, so that the product can not flow at high temperature, can still keep the original form after being cooled, and can be repeatedly heated and cooled for use.
In conclusion, the phase-change energy-storage heat-conducting material prepared by the method has good stability, and the product does not flow and deform when the temperature is repeatedly increased and decreased above and below the phase-change point.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (6)
1. The phase-change energy-storage heat-conducting material is characterized by comprising the following raw material components in parts by weight: 8-32 parts of liquid silicon rubber, 2-10 parts of zeolite molecular sieve, 30-35 parts of phase-change paraffin and 20-30 parts of spherical boron nitride;
the phase change paraffin comprises, by weight, 40% -60% of a vinyl-containing thermoplastic resin and 40% -60% of a thermoplastic hydrogenated resin;
thethermoplasticresincontainingvinylisPCM-A-44HofGuangzhouZhongjianewmaterialtechnologyCo.,Ltd; the thermoplastic hydrogenated resin is R1090 of Izeman; the liquid silicone rubber is RH-G7-1011 of Zhejiang Rudder organosilicon;
the vinyl-containing thermoplastic resin and hydrogen-containing silicone oil in the liquid silicone rubber undergo a crosslinking reaction;
the spherical boron nitride is graded spherical boron nitride, and the graded spherical boron nitride is a secondary grading system formed by spherical boron nitride with two different particle sizes;
the preparation process of the phase-change energy-storage heat-conducting material comprises the steps of uniformly mixing 8-32 parts by weight of liquid silicon rubber, 2-10 parts by weight of zeolite molecular sieve, 30-35 parts by weight of phase-change paraffin and 20-30 parts by weight of spherical boron nitride to obtain an intermediate product; adding a catalyst into the intermediate product, reacting to obtain a pre-product, and cooling the pre-product to obtain the phase-change energy storage heat-conducting material;
the catalyst is a platinum catalyst;
the reaction conditions are as follows: the temperature is 130-140 ℃ and the time is 0.5-3h.
2. The phase-change energy-storage heat-conducting material according to claim 1, wherein the zeolite molecular sieve is 250-350 mesh particles.
3. A process for preparing a phase change energy storage heat conductive material as claimed in claim 1 or 2, comprising the steps of:
according to parts by weight, uniformly mixing 8-32 parts of liquid silicone rubber, 2-10 parts of zeolite molecular sieve, 30-35 parts of phase-change paraffin and 20-30 parts of spherical boron nitride to obtain an intermediate product; and
and adding a catalyst into the intermediate product, reacting to obtain a pre-product, and cooling the pre-product to obtain the phase-change energy storage heat-conducting material.
4. The process for preparing the phase-change energy-storage heat-conducting material according to claim 3, wherein the liquid silicon rubber, the zeolite molecular sieve, the phase-change paraffin and the spherical boron nitride are uniformly stirred at the temperature of 55-65 ℃ to obtain an intermediate product.
5. The process for preparing a phase-change energy-storage heat-conducting material according to claim 3, wherein the mass ratio of the catalyst to the intermediate product is (0.01-0.2): 100.
6. the process for preparing a phase-change energy-storage heat-conducting material according to claim 3, wherein the cooling of the pre-product is specifically cooling the pre-product to room temperature.
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| CN102408877B (en) * | 2011-07-12 | 2014-03-12 | 北京化工大学 | Phase-transition composite material, preparation method and application thereof |
| CN103849356A (en) * | 2014-03-20 | 2014-06-11 | 中国电子科技集团公司第三十三研究所 | Electrical insulating phase-change heat conducting material and preparation method thereof |
| CN107746645B (en) * | 2017-11-09 | 2020-05-29 | 安徽本雅明涂料有限公司 | Weather-resistant exterior wall thermal insulation coating and preparation method thereof |
| CN109749714A (en) * | 2019-01-23 | 2019-05-14 | 深圳航美新材料科技有限公司 | A kind of high enthalpy phase-change heat silicon cream and preparation method thereof |
| CN112574568B (en) * | 2019-09-30 | 2022-12-30 | 广州玖盈化工材料有限公司 | Phase-change temperature-control silicone rubber composition and preparation method thereof |
| CN113956852A (en) * | 2021-10-11 | 2022-01-21 | 广东工业大学 | Heat-conducting phase-change gel material, preparation method thereof and battery module |
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