CN103265933A - Phase-change paraffin microcapsules for battery heat management and preparation method thereof - Google Patents
Phase-change paraffin microcapsules for battery heat management and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of storage batteries, and relates to the field of battery heat management based on phase-change materials, particularly phase-change paraffin microcapsules for battery heat management and a preparation method thereof. The phase-change paraffin microcapsules are in a shell structure, wherein the outer shell is coated on the inner core; the outer shell is composed of a styrene-methyl methacrylate copolymer; and the inner core is composed of a paraffin organic solid-liquid phase-change material. The preparation method comprises the following steps: proportionally measuring the raw materials, preparing the styrene-methyl methacrylate copolymer, adding a cosolvent, an emulsifier and the paraffin organic solid-liquid phase-change material to carry out homogenization and emulsification, stirring at constant temperature, and carrying out vacuum drying to obtain the target product. The preparation method provided by the invention has the advantages of simpleness, low cost and high yield, and is convenient for mass synthesis; and the prepared phase-change paraffin microcapsules have favorable heat accumulation property, can greatly lower the operating cost of the battery heat management system, and can not have the problems of leakage and volume expansion of the phase-change material.
Description
Technical field
The invention belongs to the store battery field, relate to the battery thermal management field based on phase change material, relate in particular to phase transformation paraffin microcapsule for battery thermal management and preparation method thereof.
Background technology
Because energy shortage and environmental pollution are serious, electromobile and hybrid vehicle enjoy current new energy field to pay close attention to, and power cell equipment is the most key parts of electromobile and hybrid vehicle, and its dynamic property, life-span etc. have determined cost and the performance of whole vehicle.Battery use optimum temps be 10 ~ 50 ℃, battery pile is carried out in the discharge process of actual motion, the temperature that produces but can be up to more than 100 ℃, the temperature that causes of charge and discharge process is unbalanced in addition, these all are the major causes that causes series of cells to lose efficacy.Therefore, the battery management system that comprises the heat management unit becomes and determines electromobile and the business-like gordian technique of hybrid power automobile battery.
No matter be from technical standpoint energy-conservation, that improve the vehicle continual mileage, still from the miniaturization of vehicle, microminiaturized trend, traditional is that the heat management system of heat-eliminating medium all makes total system heaviness, complexity with air, water.In recent years, the heat management system of employing phase change material has caused the concern of many electromobile production firms and battery manufacturers.Application publication number is that the Chinese invention patent of CN102364747A discloses a kind of battery temp management system based on phase change material.Application publication number is that the Chinese invention patent of CN102181270A discloses and a kind ofly meets phase change material and device for lithium cell heat radiation.Application publication number is that U.S.'s patent of invention of CN1418373A discloses a kind of equipment for passive phase change thermal management and method.Application publication number is a kind of composite phase-change material and device for the silica-based solar cell heat radiation of the Chinese invention patent of CN102509741A.These patents have all proposed to utilize phase change material that energy storage system is carried out heat management, the phase change material that relates to mainly is paraffin, aliphatic saturated hydrocarbon etc., because phase change material such as paraffin has problems such as the leakage of liquid and volumetric expansion when undergoing phase transition, thereby reduce the battery heat dispersion, influence dynamic property and the life-span of battery.
Summary of the invention
Occur easily when the objective of the invention is to overcome phase change material and undergoing phase transition leaking and the problem of volumetric expansion, a kind of phase transformation paraffin microcapsule for battery thermal management and preparation method thereof is provided, this preparation method is simple to operate, cost is low, the productive rate height is convenient to a large amount of synthesizing, and the phase transformation paraffin microcapsule heat storage performance for preparing is good, can reduce the running cost of battery thermal management system greatly, the problem of phase change material leakage and volumetric expansion can not occur.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of phase transformation paraffin microcapsule for battery thermal management, described phase transformation paraffin microcapsule is shell structure, outer shell parcel inner sandwich layer, described outer shell is to be made of vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer, described inner sandwich layer is to be made of the organic solid-liquid phase change material of paraffin class.
Series of cells is immersed in the phase transformation paraffin microcapsule, absorb the battery liberated heat and battery temperature is reduced rapidly as the organic solid-liquid phase change material of the paraffin class of inner sandwich layer, the organic solid-liquid phase change material of paraffin class undergoes phase transition after absorbing the battery liberated heat, becomes liquid from solid state transformation.But, owing to be used as the vinylbenzene of outer shell-methylbenzene olefin(e) acid methyl terpolymer parcel and can't flow out, so integral body leakage and the volumetric expansion phenomenon of phase change material can not appear in dispersed fine between the phase transformation paraffin microcapsule particle.
Preferably, the mass percent of the organic solid-liquid phase change material of material paraffin class of the material of described outer shell vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer and inner sandwich layer is 1:0.8 ~ 2.
A kind of preparation method of the phase transformation paraffin microcapsule for battery thermal management, step is as follows:
The first step is 1:2 by mass ratio, gets vinylbenzene, methylbenzene olefin(e) acid methyl esters; And get initiator according to 0.5% of above-mentioned raw materials total mass, described initiator is: Diisopropyl azodicarboxylate or dibenzoyl peroxide;
Second step, above-mentioned raw materials and initiator are joined in the reaction vessels, it is in the nitrogen environment, and successively at 80 ℃ of thermostatically heating 30 ~ 50min, 60 ℃ of thermostatically heating 3 ~ 5h and 100 ℃ of thermostatically heating 1 ~ 2h, obtains vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer;
The 3rd goes on foot, and measures the cosolvent of the second step products therefrom quality 600 ~ 1400%, joins in the second step products therefrom, and fully dissolving obtains solution A, and described cosolvent is: ethyl acetate or methylene dichloride;
The 4th step, by the second step products therefrom quality 80 ~ 200%, take by weighing the organic solid-liquid phase change material of paraffin class and heating and melting after, mix with the 3rd step gained solution A, obtain solution B;
The 5th step, measure the emulsifying agent of the second step products therefrom quality 2%～8%, to the deionized water that wherein adds the second step products therefrom quality 1500-2500%, be heated to emulsifiers dissolve, obtain the composite emulsifying agent solution, described emulsifying agent is: the mixture of one or more in tween-80, polyvinyl alcohol solution or the styrene-maleic anhydride copolymer; The 6th step, the 4th step gained solution B is mixed with the 5th step gained composite emulsifying agent solution, homogenizing emulsifying obtains white emulsion;
In the 7th step, the 6th step gained white emulsion is stirred to cosolvent finishes evaporation under 35-45 ℃;
The 8th step, the 7th step products therefrom is carried out vacuum filtration, drying, namely get the phase transformation paraffin microcapsule for battery thermal management.
Preferably, among the described preparation method, the reaction vessels described in second step is the single port flask.
Preferably, among the described preparation method, in second step, the device that thermostatically heating is used is respectively the thermostat water bath of 80 ℃, 60 ℃ and 100 ℃; In the 7th step, the 6th step gained white emulsion is stirred in 40 ℃ thermostat water bath.
Preferably, among the described preparation method, in second step, described raw material and initiator are successively at 80 ℃ of thermostatically heating 40min, 60 ℃ of thermostatically heating 4h and 100 ℃ of thermostatically heating 1.5h.
Preferably, among the described preparation method, in the 3rd step, the consumption of cosolvent is 800% of the second step products therefrom quality.
Preferably, among the described preparation method, in the 4th step, by 150% of the second step products therefrom quality, take by weighing the organic solid-liquid phase change material of paraffin class.
Preferably, among the described preparation method, in the 5th step, measure 5% emulsifying agent of the second step products therefrom quality, to the deionized water that wherein adds the second step products therefrom quality 2000%.
Preferably, among the described preparation method, in the 5th step, serve as emulsifying agent or for the mass percent of the polyvinyl alcohol solution of component in the emulsifying agent be 5%.
The present invention compared with prior art has following advantage:
1. the preparation method of the present invention's employing has adopted phase separation method, and is simple to operate, simple equipments, and the productive rate height, cost is low, is applicable to scale operation.
2. the present invention prepares the phase transformation paraffin microcapsule for battery thermal management, be difficult for when undergoing phase transition leaking and volumetric expansion, can be widely used in battery thermal management system, replacing traditional air or water is the heat management of heat-eliminating medium, temperature when reducing battery operation has greatly guaranteed performance and the life-span of battery.
Description of drawings
Fig. 1 is preparation technology's schema of product in the embodiment of the invention 1;
Fig. 2 is the cross-sectional view of the phase transformation paraffin microcapsule of preparation in the embodiment of the invention 1;
Fig. 3 is that the phase transformation paraffin microcapsule of preparation in the embodiment of the invention 1 is at the observation figure of microscopically;
Fig. 4 is the differential scanning calorimetric figure of the phase transformation paraffin microcapsule of preparation in the embodiment of the invention 1.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Embodiment 1
The first step takes by weighing vinylbenzene 2.00g, methylbenzene olefin(e) acid methyl esters 4.00g; Take by weighing Diisopropyl azodicarboxylate 0.03g;
Second step, vinylbenzene, methyl methacrylate, the Diisopropyl azodicarboxylate that takes by weighing joined in the single port flask, and after being placed in the nitrogen environment, place 80 ℃, 60 ℃ and 100 ℃ of thermostat water baths successively, carry out 60 ℃ of thermostatically heating of 80 ℃ of thermostatically heating, 3h of 30min and 100 ℃ of thermostatically heating of 1h respectively, reaction obtains vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer;
The 3rd goes on foot, and measures the ethyl acetate of 40mL, joins in the multipolymer of the second step gained, fully after the dissolving, obtains solution A;
The 4th step, by 80% of the second step gained copolymer quality, take by weighing paraffin phase change material and heating and melting after, mix with the 3rd step gained solution A, obtain solution B;
The 5th step, get 0.05g tween-80,0.055g styrene-maleic anhydride copolymer and 7mL mass percent and be 0.5% polyvinyl alcohol, to wherein adding the 90mL deionized water, be heated to dissolving, obtain the composite emulsifying agent solution;
The 6th step, the 4th step gained solution B is mixed with the 5th step gained composite emulsifying agent solution, homogenizing emulsifying obtains white emulsion;
The 7th step was stirred to cosolvent with the 6th step gained white emulsion and finishes evaporation in 35 ℃ thermostat water bath, form the microcapsule of ad hoc structure thereby be separated;
The 8th step, the 7th step products therefrom is carried out vacuum filtration, drying, namely get the phase transformation paraffin microcapsule for battery thermal management.
As shown in Figure 2, Fig. 2 is the sectional view of the phase transformation paraffin microcapsule that is used for battery thermal management of preparation gained in the present embodiment, the outer shell 1 parcel inner sandwich layer 2 of phase transformation paraffin microcapsule.The material of outer shell 1 is vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer, and the material of inner sandwich layer 2 is paraffin phase change material.
As shown in Figure 3, Fig. 3 is that the phase transformation paraffin microcapsule that is used for battery thermal management of preparation gained in the present embodiment is schemed in microscope observation, and the microcapsule dispersiveness of preparing is fine, and obvious shell structure is arranged.
As shown in Figure 4, Fig. 4 is the differential scanning calorimetric figure of the phase transformation paraffin microcapsule that is used for battery thermal management of preparation gained in the present embodiment, be the numerical value of suction heat release of the product of the present embodiment preparation that under the situation of constant temperature rise rate, records, the transformation temperature of each peak value place counter sample of this figure.
Series of cells is immersed in the phase transformation paraffin microcapsule of present embodiment preparation, absorb the battery liberated heat and battery temperature is reduced rapidly as the organic solid-liquid phase change material of the paraffin class of inner sandwich layer 2, the organic solid-liquid phase change material of paraffin class is after absorbing the battery liberated heat, undergo phase transition, become liquid from solid state transformation, but can't flow out owing to be used as the vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer parcel of outer shell 1, so dispersed fine between the phase transformation paraffin microcapsule particle, the integral body that phase change material can not occur is leaked and the volumetric expansion phenomenon.
Embodiment 2
The first step takes by weighing vinylbenzene 2.00g, methylbenzene olefin(e) acid methyl esters 4.00g; Take by weighing Diisopropyl azodicarboxylate 0.03g;
Second step, vinylbenzene, methyl methacrylate, the Diisopropyl azodicarboxylate that takes by weighing joined in the single port flask, and after being placed in the nitrogen environment, place 80 ℃, 60 ℃ and 100 ℃ of thermostat water baths successively, carry out 60 ℃ of thermostatically heating of 80 ℃ of thermostatically heating, 5h of 50min and 100 ℃ of thermostatically heating of 1.5h respectively, reaction obtains vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer;
The 3rd goes on foot, and measures the ethyl acetate of 90mL, joins in the multipolymer of the second step gained, fully after the dissolving, obtains solution A;
The 4th step, by 200% of the second step gained copolymer quality, take by weighing paraffin phase change material and heating and melting after, mix with the 3rd step gained solution A, obtain solution B;
The 5th step, get 0.025g tween-80,0.02g styrene-maleic anhydride copolymer and 15mL mass percent and be 0.5% polyvinyl alcohol, to wherein adding the 150mL deionized water, be heated to dissolving, obtain the composite emulsifying agent solution;
The 6th step, the 4th step gained solution B is mixed with the 5th step gained composite emulsifying agent solution, homogenizing emulsifying obtains white emulsion;
The 7th step was stirred to cosolvent with the 6th step gained white emulsion and finishes evaporation in 45 ℃ thermostat water bath, form the microcapsule of ad hoc structure thereby be separated;
The 8th step, the 7th step products therefrom is carried out vacuum filtration, drying, namely get the phase transformation paraffin microcapsule for battery thermal management.
The first step takes by weighing vinylbenzene 2.00g, methylbenzene olefin(e) acid methyl esters 4.00g; Take by weighing Diisopropyl azodicarboxylate 0.03g;
Second step, vinylbenzene, methyl methacrylate, the Diisopropyl azodicarboxylate that takes by weighing joined in the single port flask, and after being placed in the nitrogen environment, place 80 ℃, 60 ℃ and 100 ℃ of thermostat water baths successively, carry out 60 ℃ of thermostatically heating of 80 ℃ of thermostatically heating, 4h of 40min and 100 ℃ of thermostatically heating of 1.5h respectively, reaction obtains vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer;
The 3rd goes on foot, and measures the ethyl acetate of 55mL, joins in the multipolymer of the second step gained, fully after the dissolving, obtains solution A;
The 4th step, by 150% of the second step gained copolymer quality, take by weighing paraffin phase change material and heating and melting after, mix with the 3rd step gained solution A, obtain solution B;
The 5th step, get 0.01g tween-80,0.015g styrene-maleic anhydride copolymer and 15mL mass percent and be 0.5% polyvinyl alcohol, to wherein adding the 120mL deionized water, be heated to dissolving, obtain the composite emulsifying agent solution;
The 6th step, the 4th step gained solution B is mixed with the 5th step gained composite emulsifying agent solution, homogenizing emulsifying obtains white emulsion;
The 7th step was stirred to cosolvent with the 6th step gained white emulsion and finishes evaporation in 40 ℃ thermostat water bath, form the microcapsule of ad hoc structure thereby be separated;
The 8th step, the 7th step products therefrom is carried out vacuum filtration, drying, namely get the phase transformation paraffin microcapsule for battery thermal management.
Claims (10)
1. phase transformation paraffin microcapsule that is used for battery thermal management, it is characterized in that: described phase transformation paraffin microcapsule is shell structure, outer shell parcel inner sandwich layer, described outer shell is to be made of vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer, and described inner sandwich layer is to be made of the organic solid-liquid phase change material of paraffin class.
2. the phase transformation paraffin microcapsule for battery thermal management as claimed in claim 1, it is characterized in that: the mass percent of the material vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer of described outer shell and the organic solid-liquid phase change material of material paraffin class of inner sandwich layer is 1:0.8 ~ 2.
3. the preparation method of the phase transformation paraffin microcapsule for battery thermal management as claimed in claim 1 is characterized in that step is as follows:
The first step is 1:2 by mass ratio, gets vinylbenzene, methylbenzene olefin(e) acid methyl esters; And get initiator according to 0.5% of above-mentioned raw materials total mass, described initiator is: Diisopropyl azodicarboxylate or dibenzoyl peroxide;
Second step, above-mentioned raw materials and initiator are joined in the reaction vessels, it is in the nitrogen environment, and successively at 80 ℃ of thermostatically heating 30 ~ 50min, 60 ℃ of thermostatically heating 3 ~ 5h and 100 ℃ of thermostatically heating 1 ~ 2h, obtains vinylbenzene-methylbenzene olefin(e) acid methyl terpolymer;
The 3rd goes on foot, and measures the cosolvent of the second step products therefrom quality 600 ~ 1400%, joins in the second step products therefrom, and fully dissolving obtains solution A, and described cosolvent is: ethyl acetate or methylene dichloride;
The 4th step, by the second step products therefrom quality 80 ~ 200%, take by weighing the organic solid-liquid phase change material of paraffin class and heating and melting after, mix with the 3rd step gained solution A, obtain solution B;
The 5th step, measure the emulsifying agent of the second step products therefrom quality 2%～8%, to the deionized water that wherein adds the second step products therefrom quality 1500-2500%, be heated to emulsifiers dissolve, obtain the composite emulsifying agent solution, described emulsifying agent is: the mixture of one or more in tween-80, polyvinyl alcohol solution or the styrene-maleic anhydride copolymer;
The 6th step, the 4th step gained solution B is mixed with the 5th step gained composite emulsifying agent solution, homogenizing emulsifying obtains white emulsion;
In the 7th step, the 6th step gained white emulsion is stirred to cosolvent finishes evaporation under 35-45 ℃;
The 8th step, the 7th step products therefrom is carried out vacuum filtration, drying, namely get the phase transformation paraffin microcapsule for battery thermal management.
4. the preparation method of the phase transformation paraffin microcapsule for battery thermal management as claimed in claim 3, it is characterized in that: the reaction vessels described in second step is the single port flask.
5. the preparation method of the phase transformation paraffin microcapsule for battery thermal management as claimed in claim 3 is characterized in that: in second step, the device that thermostatically heating is used is respectively the thermostat water bath of 80 ℃, 60 ℃ and 100 ℃; In the 7th step, the 6th step gained white emulsion is stirred in 40 ℃ thermostat water bath.
6. as the preparation method of claim 3 or 5 arbitrary described phase transformation paraffin microcapsules for battery thermal management, it is characterized in that: in second step, described raw material and initiator are successively at 80 ℃ of thermostatically heating 40min, 60 ℃ of thermostatically heating 4h and 100 ℃ of thermostatically heating 1.5h.
7. the preparation method of the phase transformation paraffin microcapsule for battery thermal management as claimed in claim 3, it is characterized in that: in the 3rd step, the consumption of cosolvent is 800% of the second step products therefrom quality.
8. the preparation method of the phase transformation paraffin microcapsule for battery thermal management as claimed in claim 3 is characterized in that: in the 4th step, by 150% of the second step products therefrom quality, take by weighing the organic solid-liquid phase change material of paraffin class.
9. the preparation method of the phase transformation paraffin microcapsule for battery thermal management as claimed in claim 3, it is characterized in that: in the 5th step, measure 5% emulsifying agent of the second step products therefrom quality, to the deionized water that wherein adds the second step products therefrom quality 2000%.
10. the preparation method of the phase transformation paraffin microcapsule for battery thermal management as claimed in claim 3 is characterized in that: in the 5th step, serve as emulsifying agent or for the mass percent of the polyvinyl alcohol solution of component in the emulsifying agent be 5%.
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| CN108682919A (en) * | 2018-05-18 | 2018-10-19 | 中国科学院广州能源研究所 | A kind of system and method for the Li-ion batteries piles heat management based on phase-change microcapsule suspension |
| CN110600168A (en) * | 2019-09-16 | 2019-12-20 | 山东大学 | Liquid cooling charging cable and cooling system applied to electric automobile rapid charging |
| CN112336651A (en) * | 2020-12-10 | 2021-02-09 | 广州市柏菲化妆品有限公司 | Hejoba moisturizing membrane and preparation method thereof |
| CN113861942A (en) * | 2021-09-14 | 2021-12-31 | 中北大学 | Organic-microcapsule phase change material, preparation method thereof and application thereof in battery thermal management system |
| CN115386344A (en) * | 2021-05-25 | 2022-11-25 | 中国石油天然气股份有限公司 | Paraffin-based composite phase change microcapsule and preparation method thereof |
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| CN108682919A (en) * | 2018-05-18 | 2018-10-19 | 中国科学院广州能源研究所 | A kind of system and method for the Li-ion batteries piles heat management based on phase-change microcapsule suspension |
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| CN110600168B (en) * | 2019-09-16 | 2020-08-28 | 山东大学 | Liquid cooling charging cable and cooling system applied to electric automobile rapid charging |
| CN112336651A (en) * | 2020-12-10 | 2021-02-09 | 广州市柏菲化妆品有限公司 | Hejoba moisturizing membrane and preparation method thereof |
| CN115386344A (en) * | 2021-05-25 | 2022-11-25 | 中国石油天然气股份有限公司 | Paraffin-based composite phase change microcapsule and preparation method thereof |
| CN113861942A (en) * | 2021-09-14 | 2021-12-31 | 中北大学 | Organic-microcapsule phase change material, preparation method thereof and application thereof in battery thermal management system |
| CN113861942B (en) * | 2021-09-14 | 2024-05-03 | 中北大学 | Organic-microcapsule phase change material, preparation method thereof and application thereof in battery thermal management system |
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Application publication date: 20130828 |