CN110218326A - A kind of block aeroge, preparation method and application - Google Patents
A kind of block aeroge, preparation method and application Download PDFInfo
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- CN110218326A CN110218326A CN201910501096.2A CN201910501096A CN110218326A CN 110218326 A CN110218326 A CN 110218326A CN 201910501096 A CN201910501096 A CN 201910501096A CN 110218326 A CN110218326 A CN 110218326A
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- aeroge
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- block aeroge
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- 238000002360 preparation method Methods 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 21
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000000178 monomer Substances 0.000 claims abstract description 18
- 150000001282 organosilanes Chemical class 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 25
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 14
- 229910000077 silane Inorganic materials 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 7
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 7
- -1 aminopropyl Chemical group 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 4
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 4
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 claims description 3
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 239000002918 waste heat Substances 0.000 claims description 2
- DRUOQOFQRYFQGB-UHFFFAOYSA-N ethoxy(dimethyl)silicon Chemical compound CCO[Si](C)C DRUOQOFQRYFQGB-UHFFFAOYSA-N 0.000 claims 1
- 239000011162 core material Substances 0.000 abstract description 39
- 230000009466 transformation Effects 0.000 abstract description 39
- 229920000734 polysilsesquioxane polymer Polymers 0.000 abstract description 16
- 239000012782 phase change material Substances 0.000 abstract description 15
- 239000004964 aerogel Substances 0.000 abstract description 13
- 238000005538 encapsulation Methods 0.000 abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 description 58
- 230000008859 change Effects 0.000 description 57
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 11
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 9
- 238000002604 ultrasonography Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 6
- 238000000113 differential scanning calorimetry Methods 0.000 description 6
- 230000007704 transition Effects 0.000 description 6
- 239000012876 carrier material Substances 0.000 description 5
- 238000004378 air conditioning Methods 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- GLISOBUNKGBQCL-UHFFFAOYSA-N 3-[ethoxy(dimethyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(C)CCCN GLISOBUNKGBQCL-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 150000005846 sugar alcohols Polymers 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 210000000232 gallbladder Anatomy 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- YAQXGBBDJYBXKL-UHFFFAOYSA-N iron(2+);1,10-phenanthroline;dicyanide Chemical compound [Fe+2].N#[C-].N#[C-].C1=CN=C2C3=NC=CC=C3C=CC2=C1.C1=CN=C2C3=NC=CC=C3C=CC2=C1 YAQXGBBDJYBXKL-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 229940038384 octadecane Drugs 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- 229940094989 trimethylsilane Drugs 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Silicon Polymers (AREA)
Abstract
The present embodiments relate to nano-composite phase-changing material fields, and in particular to a kind of block aeroge, preparation method and application.The preparation method of block aeroge provided by the invention, using terephthalaldehyde and organosilane monomers as raw material, synthesize bridged polysilsesquioxane presoma, through solvent-thermal method, complicated solvent swap step is not needed, bridged polysilsesquioxane aerogel, i.e. block aeroge can be obtained through constant pressure and dry；Bridged polysilsesquioxane aerogel obtained can be used as the carrier encapsulation phase transformation core material of phase-change material, and big to the encapsulation amount of phase transformation core material in blocky, porous structure.The phase-change material that carrier encapsulation phase transformation core material obtains is done using the block aeroge, the problems such as core material leakage can effectively be solved, mutually separate and corrode, it can be used for electric vehicle battery system, effectively absorb the amount of heat generated in electric car use process, meet winter car heating demands.
Description
Technical field
The present invention relates to nano-composite phase-changing material fields, and in particular to a kind of block aeroge, preparation method and answers
With.
Background technique
As the problems such as energy shortage and environmental pollution increasingly sharpens, in recent years, environment-friendly and energy-efficient pure electric automobile is by people
Extensive concern, use it is more and more.Power resources of the battery as electric car, on the one hand, since electric car works
The limitation of principle, winter do not have the circulating cooling liquid of engine to carry out heat supply, and interior heating, air-conditioning system can only be carried out by electric heating
The high electric energy consumption of system causes electric car cruising ability to be greatly lowered；On the other hand, since battery high-intensity discharge can source
Source is constantly be generated a large amount of heat, and the heat of generation directly affects the performance of battery, service life, durability.Therefore, research lithium electricity
The heat management in pond and heat utilization are highly important with the normal work for guaranteeing battery.
Phase-change material can absorb or discharge a large amount of latent heat in phase transition process, there is important answer in terms of energy stores
With.Select a kind of energy storage density big, light weight, the high phase-change material of thermal stability is used for more than power battery thermal management system recycling
Heat is simultaneously stored, and can guarantee that battery works under normal operational temperature conditions, while can be with when needing heat
It discharges heat to heat for winter car, maintains automobile course continuation mileage to reduce air-conditioning system power consumption.But there has been no can
Meet the phase-change material of power battery thermal management system requirement well.In addition, the preparation method of existing phase-change material, is two steps
Method is first made carrier material, then uses carrier adsorption phase transformation core material, so that obtained phase-change material, complex steps are uncontrollable.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
Goal of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of block aeroges, block aeroge phase transformation
Composite material, preparation method and application.The preparation method of block aeroge provided by the invention, with terephthalaldehyde and organic
Silane monomer is Material synthesis bridged polysilsesquioxane presoma, and the poly- sesquialter silicon of bridging can be obtained through solvent-thermal method and drying
Oxygen alkane aeroge, i.e. block aeroge；Bridged polysilsesquioxane aerogel obtained can be used as phase in blocky, porous structure
Become the carrier encapsulation phase transformation core material of material, and big to the encapsulation amount of phase transformation core material.Block aeroge phase transformation provided by the invention is multiple
The preparation method of condensation material is added using the block aeroge as carrier material in the initial phase for preparing block aeroge
Phase transformation core material, the preparation of aeroge and the encapsulation of phase transformation core material carry out simultaneously, and to obtain the final product, preparation method is simple, quick for a step.This hair
Block aeroge phase change composite material made from the preparation method of the block aeroge phase change composite material of bright offer is a kind of new
Type phase-change material has good hot property and stability, also has certain heat-proof quality, temperature control range is constant, and can have
The problems such as effect solves core material leakage, mutually separates and corrode, realizes the integration of thermal energy storage and temperature regulation.Preparation of the invention
Block aeroge phase change composite material made from method can be used for electric vehicle battery system, can effectively absorb electric car use
The amount of heat generated in the process meets winter car heating demands, and solving the high electric energy consumption of air-conditioning system causes course continuation mileage to subtract
Few problem.
Solution
Purpose to realize the present invention, the embodiment of the invention provides a kind of preparation method of block aeroge, the preparations
Method includes:
Terephthalaldehyde and organosilane monomers are added into solvent；Solvent-thermal method obtains gel rubber material；It is dry, obtain bridge
Join polysilsesquioxane aerogel, i.e. block aeroge.
In one possible implementation, the preparation method includes: to molten to the preparation method of above-mentioned block aeroge
Terephthalaldehyde, organosilane monomers and silane co-precursor are added in agent.
In one possible implementation, solvent-thermal method reaction temperature is 100- to the preparation method of above-mentioned block aeroge
150 DEG C, it is optionally 120 DEG C；Reaction time is 20-28h.
In one possible implementation, drying temperature is 70-80 DEG C to the preparation method of above-mentioned block aeroge；It is dry
Time is 40-48h.
The preparation method of above-mentioned block aeroge in one possible implementation, terephthalaldehyde and organosilan list
The molar ratio of body is 1:1.8-2.3.
In one possible implementation, organosilane monomers include: 3- ammonia to the preparation method of above-mentioned block aeroge
Base propyl-triethoxysilicane (No. CAS is 919-30-2), (No. CAS is 13822-56- to 3- TSL 8330
5), (3- aminopropyl)-diethoxymethylsilane (No. CAS is 3179-76-8), (3- aminopropyl) dimethylethyloxy silicon
At least one of alkane (No. CAS is 18306-79-1).
In one possible implementation, silane co-precursor includes methyl three to the preparation method of above-mentioned block aeroge
Methoxy silane (No. CAS is 1185-55-3), tetraethoxysilane (No. CAS is 78-10-4), methyltriethoxysilane
(No. CAS is 2031-67-6), trimethoxy propyl silane (No. CAS is 1067-25-0), methoxytrimethylsilane (No. CAS
For at least one of 1825-61-2).
The embodiment of the invention also provides block aeroges made from the preparation method of above-mentioned block aeroge.
The embodiment of the invention also provides a kind of preparation method of block aeroge phase change composite material, the preparation methods
Include:
Phase transformation core material, terephthalaldehyde and organosilane monomers are added into solvent；Solvent-thermal method obtains gel rubber material；It is dry
It is dry, obtain block aeroge phase change composite material.
Wherein, organosilane monomers include the methyl-monosilane of organic bridge linkage group and functionalization.Two in terephthalaldehyde
A aldehyde groups can be reacted with the amino group in organosilane monomers, bridged polysilsesquioxane presoma be synthesized, through solvent
After thermal method and drying, blocky porous bridged polysilsesquioxane aerogel can be obtained.In addition, preparing the poly- sesquialter silicon of bridging
Phase transformation core material is added when oxygen alkane aeroge, it can be achieved that the preparation of aeroge and one step of the encapsulation completion of phase transformation core material, obtain
Block aeroge phase change composite material is the porous bridged polysilsesquioxane aerogel of bulk for encapsulating phase transformation core material.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, the preparation side
Method includes: that phase transformation core material, terephthalaldehyde, organosilane monomers and silane co-precursor are added into solvent.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, the preparation side
Method includes: the phase transition temperature that drying temperature is higher than phase transformation core material.
In one possible implementation, solvent is second to the preparation method of above-mentioned block aeroge phase change composite material
Alcohol.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, the preparation side
Method includes the following steps:
Terephthalaldehyde and phase transformation core material are dissolved in ethyl alcohol, ultrasound；Then organosilane monomers are added, ultrasound；It adds
Deionized water, ultrasonic disperse are transferred in reaction kettle；
Reaction kettle is placed in baking oven and is reacted, gel rubber material is obtained；
The taking-up of reaction kettle liner is placed in oven and dried, block aeroge phase change composite material is obtained；Wherein, dry temperature
Degree is higher than the phase transition temperature of phase transformation core material；
Optionally, silane co-precursor is additionally added in addition to organosilane monomers.The effect that deionized water is added is to promote silicon
The hydrolysis of alkane.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, when each step ultrasound
Power be 400-700W, be optionally 600W；Ultrasonic time is 5-25min.
In one possible implementation, reaction kettle is set for the preparation method of above-mentioned block aeroge phase change composite material
When reacting in baking oven, oven temperature is 100-150 DEG C, is optionally 120 DEG C；Reaction time is 20-28h.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, will be in reaction kettle
When gallbladder taking-up is placed in oven and dried, drying temperature is 70-80 DEG C；Drying time is 40-48h.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, terephthalaldehyde
Molar ratio with organosilane monomers is 1:1.8-2.3.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, phase transformation core material and
The mass ratio of aeroge carrier is 1-100:1-100；It is optionally 20-70:100；It is still optionally further 50-70:100.Its
In, aeroge carrier refers to that remaining step is all the same, but is added without bridged polysilsesquioxane airsetting made from phase transformation core material
Glue.
In one possible implementation, silane is total to forerunner to the preparation method of above-mentioned block aeroge phase change composite material
The molar ratio of body and organosilane monomers is 1-2:1；It is optionally 1:1 or 2:1.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, the addition of ethyl alcohol
Amount is 5-15mL；It is optionally 7-10mL；It is still optionally further 7.5-8mL.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, organosilan list
Body includes: 3-aminopropyltriethoxysilane, 3- TSL 8330, (3- aminopropyl)-diethoxy first
At least one of base silane, (3- aminopropyl) dimethylethoxysilane.
The preparation method of above-mentioned block aeroge phase change composite material in one possible implementation, phase transformation core material packet
It includes: at least one of polyalcohols, fatty acid, paraffin class；Optionally, it is 600- that polyalcohols, which include average molecular weight,
At least one of 10000 polyethylene glycol, pentaerythrite, neopentyl glycol；Fatty acid includes stearic acid, myristic acid, palm fibre
At least one of palmitic acid acid, capric acid, lauric acid, pentadecanoic acid, octadecyl alcolol, stearic acid, octadecylamine, octadecane.
In one possible implementation, silane is total to forerunner to the preparation method of above-mentioned block aeroge phase change composite material
Body includes methyltrimethoxysilane, tetraethoxysilane, methyltriethoxysilane, trimethoxy propyl silane, methoxyl group
At least one of trimethyl silane.
The embodiment of the invention also provides block gas made from the preparation method of above-mentioned block aeroge phase change composite material
Gel phase change composite material.
The embodiment of the invention also provides the preparation method of above-mentioned block aeroge, block aeroge, block aeroge phases
Application of the preparation method or block aeroge phase change composite material of change composite material in electric vehicle battery system.
In one possible implementation, the application includes: in electric vehicle battery system for above-mentioned application
Waste heat recycling is to be used for electric car heat supply in winter.
Beneficial effect
(1) preparation method of block aeroge provided in an embodiment of the present invention, with terephthalaldehyde and organosilane monomers
Complicated solvent swap step is not needed, is often pressed dry through solvent-thermal method for Material synthesis bridged polysilsesquioxane presoma
Dry that bridged polysilsesquioxane aerogel can be obtained, bridged polysilsesquioxane aerogel obtained is in blocky, porous structure；
It can be used as the carrier encapsulation phase transformation core material of phase-change material；And it is big to the encapsulation amount of phase transformation core material, (i.e. load capacity refers to phase to encapsulation amount
Become the mass ratio of core material and aeroge carrier material) up to 70%, when practical application, can be big according to different demands adjusting load capacity
It is small.
(2) preparation method of the block aeroge phase change composite material provided in the embodiment of the present invention, with the poly- sesquialter of bridging
Siloxanes aeroge is carrier, and phase transformation core material is added in the initial phase for preparing bridged polysilsesquioxane aerogel, can be real
The preparation of existing aeroge and one step of encapsulation of phase transformation core material are completed, and preparation method is simple, quick.
The absorption of phase transformation core material is limited in its hole using the cellular structure of bridged polysilsesquioxane aerogel carrier material
In road, effectively core material can be prevented to reveal.By adjusting the type and load capacity of phase transformation core material, can prepare a series of suitable for different works
Make the block aeroge phase change composite material of temperature.
(3) preparation method of the block aeroge phase change composite material provided in the embodiment of the present invention, while can also introduce
Different types of silane co-precursor, the silane co-precursor of introducing can improve the mechanical property of aeroge phase change composite material,
Assign aerogel material flexibility, hydrophobicity etc..
In addition, by the type and quality that change the silane co-precursor being added, the poly- sesquialter of adjustable carrier material bridging
The aperture of siloxanes aeroge, to preferably be adapted to different types of phase transformation core material.
(4) block aeroge phase change composite material made from preparation method provided by the invention, to encapsulate phase transformation core material
The porous bridged polysilsesquioxane aerogel of bulk, be a kind of new material, there is good hot property (latent heat of phase change
Height, energy storage are high) and stability, and because its thermal conductivity is low, also there is certain heat-proof quality, it can be achieved that heat-insulated and thermal energy storage
With the integration of temperature regulation.
(5) novel block aeroge phase change composite material made from preparation method provided by the invention, density is low, price at
This low, amount of heat generated when can effectively absorb electric car use process meets winter car heating demands, solves air-conditioning
The problem of high electric energy consumption of system causes course continuation mileage to reduce.
Detailed description of the invention
One or more embodiments are illustrated by the picture in corresponding attached drawing, these exemplary theorys
The bright restriction not constituted to embodiment.Dedicated word " exemplary " means " being used as example, embodiment or illustrative " herein.
Here as any embodiment illustrated by " exemplary " should not necessarily be construed as preferred or advantageous over other embodiments.
Fig. 1 is the block aeroge composite phase-change material sample drawing that the embodiment of the present invention 3 obtains.
Fig. 2 is block aeroge composite phase-change material scanning electron microscope (SEM) scanning that the embodiment of the present invention 3 obtains
Figure.
Fig. 3 is the Fourier infrared spectrograph for the block aeroge composite phase-change material that the embodiment of the present invention 3 obtains
(FTIR) map.
Fig. 4 is differential scanning calorimetry (DSC) figure for the block aeroge composite phase-change material that the embodiment of the present invention 3 obtains
Spectrum.
Fig. 5 is the load-deformation curve for the block aeroge composite phase-change material that the embodiment of the present invention 3 and 4 obtains.
Fig. 6 is the DSC map for the block aeroge composite phase-change material that the embodiment of the present invention 6 obtains.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described, it is clear that described embodiments are some of the embodiments of the present invention, rather than
Whole embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work premise
Under every other embodiment obtained, shall fall within the protection scope of the present invention.Unless otherwise explicitly stated, otherwise whole
In a specification and claims, it is to include that the term " include " or its transformations will be understood as
The element or component stated, and do not exclude other elements or other components.
In addition, in order to better illustrate the present invention, numerous details is given in specific embodiment below.
It will be appreciated by those skilled in the art that without certain details, the present invention equally be can be implemented.In some embodiments, right
It is not described in detail in raw material well known to those skilled in the art, element, method, means etc., in order to highlight master of the invention
Purport.
Raw material is commercial product in following embodiment.
Embodiment 1
A kind of preparation method of block aeroge, includes the following steps:
It weighs 0.283g (0.002mol) terephthalaldehyde to mix with 7.5mL ethyl alcohol, (refers to supersonic wave cleaning machine water at 35 DEG C
Temperature) under ultrasound 20min；
Then 1mL (0.946g, 0.0043mol) 3- aminopropyl triethoxysilane, ultrasonic 5min are added into solution；
It is eventually adding 0.25mL deionized water, ultrasonic disperse 20min is transferred in reaction kettle；Wherein, ultrasonic power is
600W；
Reaction kettle is placed in 120 DEG C of baking oven and is reacted for 24 hours, obtains gel rubber material；
It takes out reaction kettle liner to be put into baking oven, 80 DEG C of dry 48h obtain block aeroge.
Embodiment 2
It weighs 0.283g (0.002mol) terephthalaldehyde to mix with 7.5mL ethyl alcohol, (refers to supersonic wave cleaning machine water at 35 DEG C
Temperature) under ultrasound 20min；
Then 1mL (0.946g, 0.0043mol) 3- aminopropyl triethoxysilane and 0.61mL are added into solution
(0.5795g, 0.0043mol) methyltrimethoxysilane, ultrasonic 5min；
It is eventually adding 0.25mL deionized water, ultrasonic disperse 20min is transferred in reaction kettle；Wherein, ultrasonic power is
600W；
Reaction kettle is placed in 120 DEG C of baking oven and is reacted for 24 hours, obtains gel rubber material；
It takes out reaction kettle liner to be put into baking oven, 80 DEG C of dry 48h obtain block aeroge.
Embodiment 3
A kind of preparation method of block aeroge phase change composite material, includes the following steps:
0.283g (0.002mol) terephthalaldehyde, 0.75g PEG2000 are weighed, is mixed with 7.5mL ethyl alcohol, at 35 DEG C
Ultrasound 20min under (referring to supersonic wave cleaning machine water temperature)；
Then 1mL (0.946g, 0.0043mol) 3- aminopropyl triethoxysilane, ultrasonic 5min are added into solution；
It is eventually adding 0.25mL deionized water, ultrasonic disperse 20min is transferred in reaction kettle；Wherein, ultrasonic power is
600W；
Reaction kettle is placed in 120 DEG C of baking oven and is reacted for 24 hours, obtains gel rubber material；
It takes out reaction kettle liner to be put into baking oven, 80 DEG C of dry 48h obtain block aeroge phase change composite material；Its
The load capacity (quality of PEG2000/corresponding block aeroge carrier quality) of PEG2000 is 60%.
Block aeroge phase change composite material sample obtained is as shown in Figure 1；
Its scanning electron microscope (SEM) scanning figure is as shown in Figure 2；By SEM scanning figure it is found that block aeroge phase transformation is answered
Condensation material remains corresponding block aeroge primary granule (being made of the bulky grain of random primary nanoparticle and aggregation)
Pattern；Evolution of the three-dimensional netted porous structure from original rough surface to smooth surface proves that phase transformation core material loads successfully.
It is as shown in Figure 3 that its Fourier infrared spectrograph (FTIR) analyzes result；Wherein, curve " pure PEG2000 " in figure
It is the FTIR analysis result of phase transformation core material PEG2000；Curve " aerogel " is that (it is prepared block aeroge made from embodiment 1
Step is same as Example 3, and difference, which is only that, does not load phase transformation core material PEG2000) FTIR analyze result；Curve " 60%
PEG2000@aerogel " is the block aeroge phase change composite material that phase transformation core material load capacity made from embodiment 3 is 60%
FTIR analyzes result.
The results show that in corresponding block aeroge spectrogram, the symmetrical asymmetric stretching vibration of-OH occurs for FTIR analysis
In 3431cm-1Place；The stretching vibration of functional group-CH=N- appears in 1642cm-1Place；The asymmetrical stretch of Si-O-Si stretches
Vibration and bending vibration respectively with 1041cm-1、785cm-1And 461cm-1The peak value at place is corresponding；3- aminopropyl triethoxysilane
The c h bond of upper methyl and methylene respectively corresponds 2931cm-1And 2950cm-1The peak at place.
In the spectrogram of phase transformation core material PEG2000, the stretching vibration of C-O and the stretching vibration of O-H produce 1109cm respectively-1
And 3444cm-1Absorption band；In addition, in 963cm-1And 2887cm-1Place can observe-CH2The peak value of stretching vibration.
In the spectrogram of block aeroge phase change composite material obtained, 3424cm-1One bands of a spectrum at place belong to-OH and stretch vibration
Dynamic 2885cm-1Place occurs and-CH2Midplane extrusion vibrates corresponding absorption band；1112cm-1Neighbouring band is by C-O
Stretching vibration caused by.That is, not occurring new peak in the spectrum of block aeroge phase change composite material, illustrating phase transformation
The carrier of core material and phase transformation core material is physical combination, does not have chemical action between two kinds of components, can retain phase transformation core material itself
Performance.
Its differential scanning calorimetry (DSC) figure is as shown in Figure 4；DSC test result shows block aeroge phase change composite material
Phase transition temperature be 57.40/25.07 DEG C, latent heat of phase change 90.63/83.14J/g.
Embodiment 4
A kind of preparation method of block aeroge phase change composite material, includes the following steps:
0.283g (0.002mol) terephthalaldehyde, 1.125g PEG2000 are weighed, is mixed with 7.5mL ethyl alcohol, at 35 DEG C
Ultrasound 20min under (referring to supersonic wave cleaning machine water temperature)；
Then 1mL (0.946g, 0.0043mol) 3- aminopropyl triethoxysilane and 0.61mL are added into solution
(0.5795g, 0.0043mol) methyltrimethoxysilane, ultrasonic 5min；
It is eventually adding 0.25mL deionized water, ultrasonic disperse 20min is transferred in reaction kettle；Wherein, ultrasonic power is
600W；
Reaction kettle is placed in 120 DEG C of baking oven and is reacted for 24 hours, obtains gel rubber material；
It takes out reaction kettle liner to be put into baking oven, 80 DEG C of dry 48h obtain block aeroge phase change composite material；Its
The load capacity of PEG2000 is 60%.
Block aeroge phase change composite material obtained, phase transition temperature are 57.40/25.07 DEG C, and latent heat of phase change is
90.63/83.14J/g。
The load-deformation curve of block aeroge phase change composite material made from embodiment 3 and 4 is shown in Fig. 5 respectively；By Fig. 5
It is found that embodiment 4 joined block aeroge phase change composite material made from methyltrimethoxysilane co-precursor, can bear
About 45% compressive deformation, the block aeroge phase change composite material that silane co-precursor obtains, which is not added, compared with embodiment 3 (can hold
Compressive deformation by about 18%), there is better mechanical performance.The flexibility of the phase change composite material of embodiment 4, skeleton is
What the flexible molecule chain as derived from C-C sections soft provided, this facilitates it and obtains good performance in compression test.
Embodiment 5
A kind of preparation method of block aeroge phase change composite material, includes the following steps:
0.283g (0.002mol) terephthalaldehyde, 0.75g octadecyl alcolol are weighed, mixes with 7.5mL ethyl alcohol, (refers at 35 DEG C
Supersonic wave cleaning machine water temperature) under ultrasound 20min；
Then 1mL (0.946g, 0.0043mol) 3- aminopropyl triethoxysilane, ultrasonic 5min are added into solution；
It is eventually adding 0.25mL deionized water, ultrasonic disperse 20min is transferred in reaction kettle；Wherein, ultrasonic power is
600W；
Reaction kettle is placed in 120 DEG C of baking oven and is reacted for 24 hours, obtains gel rubber material；
It takes out reaction kettle liner to be put into baking oven, 80 DEG C of dry 48h obtain block aeroge phase change composite material；It ten
The load capacity of eight alcohol is 60%.
Block aeroge phase change composite material obtained, phase transition temperature are 60.30/52.10 DEG C, and latent heat of phase change is
106.38/102.31J/g。
Embodiment 6
A kind of preparation method of block aeroge phase change composite material, includes the following steps:
0.283g (0.002mol) terephthalaldehyde, 1.125g octadecyl alcolol are weighed, mixes with 7.5mL ethyl alcohol, (refers at 35 DEG C
Supersonic wave cleaning machine water temperature) under ultrasound 20min；
Then 1mL (0.946g, 0.0043mol) 3- aminopropyl triethoxysilane and 0.61mL are added into solution
(0.5795g, 0.0043mol) methyltrimethoxysilane, ultrasonic 5min；Wherein, ultrasonic power is 600W；
It is eventually adding 0.25mL deionized water, ultrasonic disperse 20min is transferred in reaction kettle；
Reaction kettle is placed in 120 DEG C of baking oven and is reacted for 24 hours, obtains gel rubber material；
It takes out reaction kettle liner to be put into baking oven, 80 DEG C of dry 48h obtain block aeroge phase change composite material；It ten
The load capacity of eight alcohol is 60%.
The DSC figure of above-mentioned block aeroge phase change composite material obtained is as shown in Figure 6；DSC test result shows, phase
Temperature is 60.13/53.13 DEG C, and latent heat of phase change is 133.94/132.93J/g.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of block aeroge, the preparation method include:
Terephthalaldehyde and organosilane monomers are added into solvent；Solvent-thermal method obtains gel rubber material；It is dry, it is poly- to obtain bridging
Silsesquioxane aeroge, i.e. block aeroge.
2. the preparation method of block aeroge according to claim 1, which is characterized in that the preparation method include: to
Terephthalaldehyde, organosilane monomers and silane co-precursor are added in solvent.
3. the preparation method of block aeroge according to claim 2, which is characterized in that silane co-precursor includes methyl
Trimethoxy silane, tetraethoxysilane, methyltriethoxysilane, trimethoxy propyl silane, methoxytrimethylsilane
At least one of.
4. the preparation method of block aeroge according to claim 1, which is characterized in that solvent-thermal method reaction temperature is
100-150℃；Reaction time is 20-28h.
5. the preparation method of block aeroge according to claim 1, which is characterized in that drying temperature is 70-80 DEG C；It is dry
The dry time is 40-48h.
6. the preparation method of block aeroge according to claim 1, which is characterized in that terephthalaldehyde and organosilan
The molar ratio of monomer is 1:1.8-2.3.
7. the preparation method of block aeroge according to claim 1, which is characterized in that organosilane monomers include: 3-
Aminopropyltriethoxywerene werene, 3- TSL 8330, (3- aminopropyl)-diethoxymethylsilane, (3-
At least one of aminopropyl) dimethylethoxysilane.
8. block aeroge made from the preparation method of the described in any item block aeroges of claim 1-7.
9. preparation method or the block aeroge according to any one of claims 8 of the described in any item block aeroges of claim 1-7
Application in electric vehicle battery system.
10. application according to claim 9, it is characterised in that: the application includes: in electric vehicle battery system
Waste heat recycling be used for electric car heat supply in winter.
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