CN103212351B - Preparation and application methods of high-heat-conductivity flame retardant phase change microcapsule - Google Patents
Preparation and application methods of high-heat-conductivity flame retardant phase change microcapsule Download PDFInfo
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- CN103212351B CN103212351B CN201310120577.1A CN201310120577A CN103212351B CN 103212351 B CN103212351 B CN 103212351B CN 201310120577 A CN201310120577 A CN 201310120577A CN 103212351 B CN103212351 B CN 103212351B
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000003063 flame retardant Substances 0.000 title claims abstract description 11
- 230000008859 change Effects 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title abstract 7
- 239000012782 phase change material Substances 0.000 claims abstract description 13
- 239000000178 monomer Substances 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004945 emulsification Methods 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 239000012188 paraffin wax Substances 0.000 claims description 7
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004020 conductor Substances 0.000 claims description 5
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- PSYGHMBJXWRQFD-UHFFFAOYSA-N 2-(2-sulfanylacetyl)oxyethyl 2-sulfanylacetate Chemical compound SCC(=O)OCCOC(=O)CS PSYGHMBJXWRQFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- ARGZBGBUZXUAHM-UHFFFAOYSA-L potassium sodium hydrogen sulfite sulfooxy sulfate Chemical compound [Na+].[K+].OS([O-])=O.OS(=O)(=O)OOS([O-])(=O)=O ARGZBGBUZXUAHM-UHFFFAOYSA-L 0.000 claims description 2
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000004806 packaging method and process Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000003999 initiator Substances 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 9
- 238000007726 management method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 206010039203 Road traffic accident Diseases 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 239000012184 mineral wax Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- SLYCYWCVSGPDFR-UHFFFAOYSA-N octadecyltrimethoxysilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OC)(OC)OC SLYCYWCVSGPDFR-UHFFFAOYSA-N 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229940079827 sodium hydrogen sulfite Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
The invention discloses preparation and application methods of a high-heat-conductivity flame retardant phase change microcapsule. The preparation method comprises the following steps of: heating the phase change material to above melting point; adding a flame retardant, a high-heat-conductivity material and a monomer; after emulsification, filling nitrogen in a reaction kettle; and dropwise adding a water soluble initiator, and reacting for a period of time to obtain the high-heat-conductivity flame retardant phase change microcapsule. The application method comprises the following steps of: filling the high-heat-conductivity flame retardant microcapsule in the middle of monomer cell and packaging by a module frame; packaging a battery module in a battery box; and coating the high-heat-conductivity flame retardant phase change microcapsule onto the inner side of the battery box. The high-heat-conductivity flame retardant phase change microcapsule provided by the invention is high in phase change heat, high in heat conductivity and high in flame retardancy.
Description
Technical field
The present invention relates to electric vehicle engineering field, particularly relate to a kind of preparations and applicatio method of high heat conductive flame-retarding phase-change microcapsule.
Background technology
Along with developing rapidly of global industry, problem of environmental pollution highlights day by day.Especially the haze sky that causes due to air pollution of China in Recent Years, damage the whole people able-bodied while, bring inconvenience also to our trip, even cause traffic accident, threat to life.Analyze through relevant expert, cause the main cause in haze sky to be exactly the discharge of vehicle exhaust.The gasoline car of current use, while the global only petroleum resources of consumption, causes very serious impact to our environment, tramples on the living environment of descendants.So development new-energy automobile replaces conventional fuel oil car extremely urgent.Electric automobile is exactly arise at the historic moment under such an enviroment.
At present, electric automobile is all being greatly developed in countries in the world, however but not accept by most people.A major reason is exactly the security that people are difficult to trust electric automobile, and several of occurring in recent years security incident allows people inspire awe even from distance especially to electric motor car.The hot issue how allowing people drive relieved electric automobile to become current.
The core of electric automobile is electrokinetic cell, and the heat management carrying out electrokinetic cell system is for the full security of electric automobile and have vital impact the service life of electrokinetic cell.Electrokinetic cell need at a temperature rather moderate and warm field is relatively uniform its performance just can better play, especially for comparatively popular lithium titanate anode system electrokinetic cell and ternary material system electrokinetic cell, the operating temperature controlling electrokinetic cell is particularly important.Traditional electrokinetic cell heat management adopts the type of cooling that is air-cooled and liquid cooling.Air-cooled equipment is slightly simple, but Inner eycle cooling effect is limited, and substantially can only play shimming effect.And outer circulation is difficult to the requirement of shelter reaching IP67, use at the environment of humidity and rainy day the danger having electric leakage.The cooling effect of liquid cooling is better, but equipment is complicated, while consume battery power, also reduces energy density.Air-cooled and liquid cooling otherwise cooling effect limited, or huge structure is complicated, and the most important thing is to fail the heat of Appropriate application electrokinetic cell, does not reach the effect of energy-saving and emission-reduction.In recent years, phase-change material cooling becomes a kind of novel type of cooling, while the heat that timely storage of power battery distributes, can discharge the heat of storage at low temperatures, placing it in the middle of battery core and box inside, just as giving each battery core, a small-sized air conditioner being installed.Ensure that the uniformity of battery core temperature, solve heat management problems simultaneously.
Adopt phase-change material to have some to report to the research that electrokinetic cell system carries out heat management, as phase-change material is placed in the middle of monomer battery core and housing by patent CN201699090U, be aided with heater and heat management is carried out to electrokinetic cell.But the heat conduction of not mentioned phase-change material used and anti-flammability.BYD company proposes a kind of method preparing the power brick with temp regulating function, and the mineral wax of phase-change material mainly phase transition temperature about about 60 DEG C that it uses, also has the organic matters such as polyalcohol in addition, but do not add highly heat-conductive material.Shuan Deng company has applied for a kind of patent of filling the heat dissipating method of phase-change material in lithium battery interior gap.For improving heat conductivility, in organic phase change material (paraffin or stearic acid list glyceride), with the addition of metallic aluminium and material with carbon element, but the anti-flammability of not mentioned phase-change material.
Summary of the invention
The technical problem that the present invention solves is to improve the heat of transformation, high-termal conductivity and anti-flammability how simultaneously.
The embodiment of the invention discloses a kind of preparation method of high heat conductive flame-retarding phase-change microcapsule, comprise the following steps:
1.1, phase-change material is heated to more than fusing point;
1.2, fire retardant is added, highly heat-conductive material and monomer;
1.3, after emulsification, in reactor, nitrogen is filled with;
1.4, drip water soluble starter, high heat conductive flame-retarding phase-change microcapsule can be obtained after one period of reaction time.
Further, as preferably, described phase-change material is the mixture of the different various alkane of phase change paraffin or fusing point.
Further, as preferably, described fire retardant is chlorinated paraffin wax.
Further, as preferably, described highly heat-conductive material is the silica dioxide granule of surperficial oleophylic, and namely surface is through long chain alkane one type of silane coupling agent, and as octadecyl trimethoxysilane, modified silica dioxide granule, particle diameter is from 20 nanometer ~ 1 micron.
Further, as preferably, described monomer is styrene and/or divinylbenzene and/or butyl acrylate and/or GDMA and/or methyl acrylate.
Further, as preferably, described water soluble starter is potassium peroxydisulfate or ammonium persulfate or potassium peroxydisulfate-sodium hydrogensulfite initator.
Further, as preferably, the described reaction time is 4-12h.
The invention also discloses a kind of using method of high heat conductive flame-retarding phase-change microcapsule, comprise the following steps:
8.1, high heat conductive flame-retarding microcapsules are filled in the centre of monomer battery core, are encapsulated by module framework;
8.2, battery modules is encapsulated in battery case;
8.3, inside battery case, high heat conductive flame-retarding phase-change microcapsule is coated.
The present invention, for the phase-change material be applied in electrokinetic cell system heat management, except having the higher heat of transformation, also has high-termal conductivity and anti-flammability.Devise a kind of electrokinetic cell system thermal management algorithm efficiently simultaneously.
Accompanying drawing explanation
When considered in conjunction with the accompanying drawings, by referring to detailed description below, more completely can understand the present invention better and easily learn wherein many adjoint advantages, but accompanying drawing described herein is used to provide a further understanding of the present invention, form a part of the present invention, schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention, wherein:
Fig. 1 is the stereoscan photograph of high heat conductive flame-retarding phase-change microcapsule.
Detailed description of the invention
With reference to Fig. 1, embodiments of the invention are described.
For enabling above-mentioned purpose, feature and advantage become apparent more, and below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
Embodiment 1
Be that 25 DEG C of heating paraffin are to 50 DEG C by 10 parts of fusing points, add the silica dioxide granule 0.5 part of surperficial oleophylic, add 0.5 part of chlorinated paraffin wax, the mixture of 3 parts of styrene and divinylbenzene, the aqueous solution of 84 parts of emulsifying agents, adds after emulsification in reactor, be warming up to 70 DEG C, pass into nitrogen, drip that 2 parts of potassium peroxydisulfates--the aqueous solution of sodium hydrogensulfite, about 1h dropwises.After reaction 10h, terminate reaction.High heat conductive flame-retarding phase-change microcapsule can be obtained after centrifugal drying.
Add in the battery modules of LiFePO4 system by 500g height heat conductive flame-retarding phase-change microcapsule, often organize module and be made up of 5 monomer battery cores, totally two groups of modules, in the gap of high heat conductive flame-retarding phase-change microcapsule between battery core.By module packaging in battery case, battery case inwall scribbles high heat conductive flame-retarding phase-change microcapsule.The multiplying power of 2C is adopted to discharge to electrokinetic cell module, the variations in temperature on monitoring battery core surface.Before and after test, the mean temperature of battery core rises to 25 DEG C by 20 DEG C, and the temperature difference of battery core is within 2 DEG C.
The electrokinetic cell system not adding high heat conductive flame-retarding phase-change microcapsule is repeated above-mentioned test, and before and after result test, the mean temperature of battery core has 20 DEG C to rise to 41 DEG C, and the maximum temperature difference of battery core is 10 DEG C.
Above result shows, it is low 16 DEG C that the electrokinetic cell system temperature rise adding high heat conductive flame-retarding phase-change microcapsule does not add, and battery core has a narrow range of temperature 8 DEG C.This High Efficiency Thermal management method makes battery performance be not fully exerted, for safety in utilization provides guarantee.
Although the foregoing describe the specific embodiment of the present invention, but those skilled in the art is to be understood that, these detailed description of the invention only illustrate, those skilled in the art, when not departing from principle of the present invention and essence, can carry out various omission, replacement and change to the details of said method and system.Such as, merge said method step, thus then belong to scope of the present invention according to the function that the method that essence is identical performs essence identical to realize the identical result of essence.Therefore, scope of the present invention is only defined by the appended claims.
Claims (5)
1. a preparation method for high heat conductive flame-retarding phase-change microcapsule, is characterized in that, comprise the following steps:
1.1, phase-change material is heated to more than fusing point;
1.2, fire retardant is added, highly heat-conductive material and monomer, wherein:
Described monomer is oil-soluble monomer;
Described fire retardant is chlorinated paraffin wax;
Described highly heat-conductive material is the silica dioxide granule of surperficial oleophylic;
1.3, after emulsification, in reactor, nitrogen is filled with;
1.4, drip water soluble starter, high heat conductive flame-retarding phase-change microcapsule can be obtained after 4-12h.
2. the preparation method of high heat conductive flame-retarding phase-change microcapsule according to claim 1, is characterized in that, described phase-change material is the mixture of the different various alkane of phase change paraffin or fusing point.
3. the preparation method of high heat conductive flame-retarding phase-change microcapsule according to claim 1, is characterized in that, described monomer is styrene and/or divinylbenzene and/or butyl acrylate and/or GDMA and/or methyl acrylate.
4. the preparation method of high heat conductive flame-retarding phase-change microcapsule according to claim 1, is characterized in that, described water soluble starter is potassium peroxydisulfate or ammonium persulfate or potassium peroxydisulfate-sodium hydrogensulfite initator.
5. an application process for high heat conductive flame-retarding phase-change microcapsule, is characterized in that, comprise the following steps:
5.1, heat conductive flame-retarding microcapsules high described in claim 1 to 7 any one are filled in the centre of monomer battery core, are encapsulated by module framework;
5.2, battery modules is encapsulated in battery case;
5.3, inside battery case, high heat conductive flame-retarding phase-change microcapsule is coated.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103464067B (en) * | 2013-08-07 | 2015-08-05 | 苏州伟纳节能科技有限公司 | A kind of flow-line equipment preparing phase-changing energy-storing microcapsules |
| CN103805142B (en) * | 2013-12-30 | 2016-11-16 | 清华大学深圳研究生院 | A kind of silicon nitride modification microcapsules of storing energy through phase change and preparation method thereof |
| CN103740337B (en) * | 2014-01-10 | 2016-04-06 | 江苏丰彩新型建材有限公司 | A kind of novel sizing phase-change material and preparation method thereof |
| CN104212416B (en) * | 2014-08-30 | 2017-04-12 | 海安南京大学高新技术研究院 | Preparation method for paraffin microcapsule phase-change material modified by graphene oxide |
| CN105895959A (en) * | 2014-11-24 | 2016-08-24 | 深圳市沃特玛电池有限公司 | Method for improving needling safety performance of lithium ion battery |
| CN105112020A (en) * | 2015-06-11 | 2015-12-02 | 宁波绿凯节能科技有限公司 | Flame-retardant microcapsule phase-change material |
| CN106469794B (en) * | 2015-08-20 | 2019-10-15 | 江苏海四达电源股份有限公司 | A kind of method of high specific energy batteries packet internal ignition resistant cooling |
| CN105542721A (en) * | 2015-12-08 | 2016-05-04 | 北京新能源汽车股份有限公司 | Flame-retardant phase-change microcapsule and preparation method and application thereof |
| CN105355824B (en) * | 2015-12-11 | 2018-07-06 | 北京新能源汽车股份有限公司 | Power battery diaphragm, preparation method thereof and power battery comprising power battery diaphragm |
| CN105969315A (en) * | 2016-04-22 | 2016-09-28 | 江苏楚汉新能源科技有限公司 | Phase change thermal conducting material for lithium ion battery and preparation method thereof |
| CN111154459B (en) * | 2020-01-20 | 2021-03-19 | 河北工业大学 | Organic-inorganic hybrid shell phase change capsule and preparation method thereof |
| CN115093832B (en) * | 2022-06-09 | 2023-07-25 | 武汉中科先进材料科技有限公司 | Preparation method of environment-friendly heat-insulating temperature-controlling flame-retardant material |
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