WO2020248830A1 - 一种块体气凝胶、块体气凝胶相变复合材料、其制备方法及应用 - Google Patents

一种块体气凝胶、块体气凝胶相变复合材料、其制备方法及应用 Download PDF

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WO2020248830A1
WO2020248830A1 PCT/CN2020/093104 CN2020093104W WO2020248830A1 WO 2020248830 A1 WO2020248830 A1 WO 2020248830A1 CN 2020093104 W CN2020093104 W CN 2020093104W WO 2020248830 A1 WO2020248830 A1 WO 2020248830A1
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phase change
aerogel
bulk
bulk aerogel
composite material
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PCT/CN2020/093104
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English (en)
French (fr)
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王戈
刘盼盼
高鸿毅
董文钧
高志猛
陈晓
李昂
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苏州阿德旺斯新材料有限公司
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Priority claimed from CN201910501096.2A external-priority patent/CN110218326B/zh
Priority claimed from CN201910500788.5A external-priority patent/CN110256695B/zh
Application filed by 苏州阿德旺斯新材料有限公司 filed Critical 苏州阿德旺斯新材料有限公司
Publication of WO2020248830A1 publication Critical patent/WO2020248830A1/zh

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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
    • C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
    • C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
    • 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
    • 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

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  • the present invention claims the priority of a Chinese patent application filed in the Chinese Patent Office with an application number of 2019105010962 and an invention title of "a bulk aerogel, its preparation method and application”. The entire content of the application is incorporated by reference In the present invention.
  • the present invention claims the priority of a Chinese patent application filed in the Chinese Patent Office with application number 2019105007885 and the title of the invention "a bulk aerogel phase change composite material, its preparation method and application", the entire content of the application Incorporated in the present invention by reference.
  • the invention relates to the field of nanocomposite phase change materials, in particular to a bulk aerogel, a bulk aerogel phase change composite material, and a preparation method and application thereof.
  • Batteries are the power source of electric vehicles.
  • On the one hand due to the limitation of the working principle of electric vehicles, there is no circulating coolant from the engine for heating in winter, and only electric heating can be used for heating in the vehicle.
  • the high electrical energy consumption of the air conditioning system leads to the battery life of electric vehicles.
  • the capacity is greatly reduced; on the other hand, due to the high-intensity discharge of the battery, a large amount of heat will be continuously generated, which directly affects the performance, life, and durability of the battery. Therefore, it is very important to study the thermal management and thermal utilization of lithium batteries to ensure the normal operation of the batteries.
  • Phase change materials can absorb or release a large amount of latent heat in the process of phase change, and have important applications in energy storage.
  • the heat can be released for heating in the car in winter to reduce the power consumption of the air conditioning system and maintain the car's cruising range. But there is no phase change material that can well meet the requirements of power battery thermal management system.
  • the existing preparation method of the phase change material is a two-step method, that is, the carrier material is first prepared, and then the carrier material is used to adsorb the phase change core material to prepare the phase change material, and the steps are complicated and uncontrollable.
  • the purpose of the present invention is to provide a bulk aerogel, a bulk aerogel phase change composite material, and a preparation method and application thereof.
  • the preparation method of bulk aerogel provided by the present invention uses terephthalaldehyde and organosilane monomers as raw materials to synthesize bridged polysilsesquioxane precursors, and can obtain bridged polysilsesquioxanes by solvothermal method and drying.
  • Semisiloxane aerogel that is, bulk aerogel
  • the prepared bridged polysilsesquioxane aerogel has a blocky and porous structure, and can be used as a carrier for phase change materials to encapsulate phase change core materials, and
  • the encapsulation of phase change core material is large.
  • the method for preparing a bulk aerogel phase change composite material provided by the present invention uses the bulk aerogel as a carrier material, and adds the phase change core material and aerogel at the initial stage of preparing the bulk aerogel.
  • the preparation and the encapsulation of the phase change core material are carried out at the same time, and the preparation method is simple and fast.
  • the bulk aerogel phase change composite material prepared by the preparation method of the bulk aerogel phase change composite material provided by the present invention is a new type of phase change material, has good thermal performance and stability, and has certain Thermal insulation performance, constant temperature control range, and can effectively solve core material leakage, phase separation and corrosion problems, and realize the integration of thermal energy storage and temperature control.
  • the bulk aerogel phase change composite material prepared by the preparation method of the present invention can be used in an electric vehicle battery system, can effectively absorb a large amount of heat generated during the use of an electric vehicle, meet the heating demand in the vehicle in winter, and solve the high electrical energy consumption of the air conditioning system Cause the problem of reduced cruising range.
  • an embodiment of the present invention provides a method for preparing a bulk aerogel, and the method includes:
  • the preparation method includes: adding terephthalaldehyde, an organosilane monomer, and a silane co-precursor to a solvent.
  • the solvothermal reaction temperature is 100-150°C, optionally 120°C; and the reaction time is 20-28h.
  • the drying temperature is 70-80°C; and the drying time is 40-48h.
  • the molar ratio of terephthalaldehyde to organosilane monomer is 1:1.8-2.3.
  • the organosilane monomer includes: 3-aminopropyltriethoxysilane (CAS No. 919-30-2), 3-aminopropyl Trimethoxysilane (CAS number 13822-56-5), (3-aminopropyl)-diethoxymethylsilane (CAS number 3179-76-8), (3-aminopropyl) dimethyl One or more of ethoxysilane (CAS No. 18306-79-1).
  • the silane co-precursor includes methyltrimethoxysilane (CAS number 1185-55-3), tetraethoxysilane (CAS number 78 -10-4), methyltriethoxysilane (CAS No. 2031-67-6), trimethoxypropylsilane (CAS No. 1067-25-0), methoxytrimethylsilane (CAS The number is one or more of 1825-61-2).
  • the embodiment of the present invention also provides a bulk aerogel prepared by the method for preparing a bulk aerogel.
  • the embodiment of the present invention also provides a preparation method of the bulk aerogel phase change composite material, the preparation method includes:
  • phase change core material terephthalaldehyde and organosilane monomer to the solvent; obtain gel material by solvothermal method; dry to obtain bulk aerogel phase change composite material.
  • the organosilane monomer includes an organic bridging group and a functionalized methylsilane.
  • the two aldehyde groups in terephthalaldehyde can react with the amino groups in the organosilane monomer to synthesize the bridged polysilsesquioxane precursor. After solvothermal method and drying, the block can be obtained Shaped porous bridged polysilsesquioxane aerogel.
  • phase change core material is added when the bridged polysilsesquioxane aerogel is prepared, and the preparation of the aerogel and the encapsulation of the phase change core material can be completed in one step, and the obtained bulk aerogel phase change composite
  • the material is a block-shaped porous bridged polysilsesquioxane aerogel encapsulating a phase change core material.
  • the preparation method of the above-mentioned bulk aerogel phase change composite material includes: adding a phase change core material, terephthalaldehyde, organosilane monomer and silane co-precursor to a solvent body.
  • the preparation method includes: the drying temperature is higher than the phase change temperature of the phase change core material.
  • the solvent is ethanol.
  • the preparation method includes the following steps:
  • a silane co-precursor is added in addition to the organosilane monomer.
  • the effect of adding deionized water is to promote the hydrolysis of silane.
  • the power during each step of ultrasound is 400-700W, optionally 600W; and the ultrasound time is 5-25min.
  • the oven temperature is 100-150°C, optionally 120°C; the reaction time is 20-28h.
  • the drying temperature is 70-80°C; the drying time is 40-48h.
  • the molar ratio of terephthalaldehyde and organosilane monomer is 1:1.8-2.3.
  • the mass ratio of the phase change core material and the aerogel carrier is 1-100:1-100; optionally 20-70: 100; further optionally 50-70:100.
  • the aerogel carrier refers to a bridged polysilsesquioxane aerogel prepared with the same other steps but without adding phase change core material.
  • the molar ratio of the silane co-precursor and the organosilane monomer is 1-2:1; alternatively, it is 1:1 or 2. :1.
  • the amount of ethanol added is 5-15 mL; optionally 7-10 mL; further optionally 7.5-8 mL.
  • the organosilane monomer includes: 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, ( One or more of 3-aminopropyl)-diethoxymethylsilane and (3-aminopropyl)dimethylethoxysilane.
  • the phase change core material includes: one or more of polyols, fatty acids, and paraffin; Alcohols include one or more of polyethylene glycol, pentaerythritol and neopentyl glycol with an average molecular weight of 600-10000; fatty acids include stearic acid, myristic acid, palmitic acid, capric acid, lauric acid, One or more of pentadecanoic acid, stearyl alcohol, stearyl acid, stearylamine, and octadecane.
  • the silane co-precursor includes methyltrimethoxysilane, tetraethoxysilane, methyltriethoxysilane, and trimethoxysilane.
  • methyltrimethoxysilane tetraethoxysilane
  • methyltriethoxysilane trimethoxysilane.
  • propylpropylsilane and methoxytrimethylsilane is one or more of propylpropylsilane and methoxytrimethylsilane.
  • the embodiment of the present invention also provides a bulk aerogel phase change composite material prepared by the method for preparing a bulk aerogel phase change composite material.
  • the embodiment of the present invention also provides a method for preparing the above-mentioned bulk aerogel, a method for preparing a bulk aerogel, a bulk aerogel phase change composite material, or a bulk aerogel phase change composite material in an electric vehicle battery system In the application.
  • the application includes: waste heat recovery in an electric vehicle battery system for heating the electric vehicle in winter.
  • the method for preparing bulk aerogels uses terephthalaldehyde and organosilane monomers as raw materials to synthesize bridged polysilsesquioxane precursors through solvothermal method without complicated
  • the bridged polysilsesquioxane aerogel can be obtained by pressing and drying frequently, and the obtained bridged polysilsesquioxane aerogel has a blocky and porous structure; it can be used as a phase change material
  • the carrier encapsulates the phase change core material; and the encapsulation amount of the phase change core material is large, and the encapsulation amount (that is, the load, refers to the mass ratio of the phase change core material to the aerogel carrier material) can reach 70%, and the actual application can be based on Different requirements adjust the size of the load.
  • the method for preparing the bulk aerogel phase change composite material uses bridged polysilsesquioxane aerogel as a carrier to prepare bridged polysilsesquioxane aerogels.
  • the phase change core material is added in the initial stage of the glue, which can realize the preparation of aerogel and the encapsulation of the phase change core material in one step, and the preparation method is simple and fast.
  • the pore structure of the bridged polysilsesquioxane aerogel carrier material is used to adsorb the phase change core material in its pores, which can effectively prevent the core material from leaking.
  • phase change core materials By adjusting the type and loading of phase change core materials, a series of bulk aerogel phase change composite materials suitable for different working temperatures can be prepared.
  • the preparation method of the bulk aerogel phase change composite material provided in the embodiment of the present invention can also introduce different kinds of silane co-precursors, and the introduced silane co-precursor can improve the aerogel phase change composite material
  • the mechanical properties of the aerogel impart flexibility and hydrophobicity to the aerogel material.
  • the pore size of the carrier material bridging polysilsesquioxane aerogel can be adjusted, so as to better adapt to different types of phase change core materials.
  • the bulk aerogel phase change composite material prepared by the preparation method provided by the present invention is a block porous bridged polysilsesquioxane aerogel that encapsulates the phase change core material, and is a new type
  • the material has good thermal properties (high phase change latent heat, high energy storage) and stability, and because of its low thermal conductivity, it also has a certain degree of heat insulation, which can realize the integration of heat insulation, thermal energy storage and temperature control ⁇ .
  • the new bulk aerogel phase change composite material prepared by the preparation method provided by the present invention has low density and low price cost, can effectively absorb a large amount of heat generated during the use of electric vehicles, and meets the heating demand in winter cars. Solve the problem that the high energy consumption of the air conditioning system leads to the reduction of the cruising range.
  • Figure 1 is a sample diagram of a bulk aerogel composite phase change material obtained in Example 3 of the present invention.
  • Example 2 is a scanning electron microscope (SEM) scanning image of the bulk aerogel composite phase change material obtained in Example 3 of the present invention.
  • Fig. 3 is a Fourier infrared spectrometer (FTIR) spectrum of the bulk aerogel composite phase change material obtained in Example 3 of the present invention.
  • FTIR Fourier infrared spectrometer
  • DSC differential scanning calorimetry
  • Fig. 5 is the stress-strain curve of the bulk aerogel composite phase change material obtained in Examples 3 and 4 of the present invention.
  • Figure 6 is a DSC chart of the bulk aerogel composite phase change material obtained in Example 6 of the present invention.
  • the raw materials in the following examples are all commercially available products.
  • a preparation method of bulk aerogel includes the following steps:
  • a preparation method of bulk aerogel includes the following steps:
  • a method for preparing a bulk aerogel phase change composite material includes the following steps:
  • the load of PEG2000 (the mass of PEG2000/the mass of the corresponding bulk aerogel carrier) is 60% .
  • the scanning electron microscope (SEM) scanning image is shown in Figure 2. From the SEM scanning image, it can be seen that the bulk aerogel phase change composite material retains the corresponding bulk aerogel original particles (all composed of random primary nanoparticles and aggregates). The morphology of the three-dimensional network porous structure from the original rough surface to the smooth surface proves that the phase change core material is successfully loaded.
  • the Fourier Infrared Spectroscopy (FTIR) analysis results are shown in Figure 3; among them, the curve “pure PEG2000” in the figure is the FTIR analysis result of the phase change core material PEG2000; the curve “aerogel” is the block prepared in Example 1.
  • the FTIR analysis results of the aerogel (the preparation steps are the same as in Example 3, except that the phase change core material PEG2000 is not loaded); the curve "60% PEG2000@aerogel” is the loading amount of the phase change core material prepared in Example 3 FTIR analysis result of 60% bulk aerogel phase change composite material.
  • a band at 3424 cm -1 belongs to the -OH tensile vibration at 2885 cm -1 and the absorption spectrum corresponding to the -CH 2 symmetric tensile vibration appears Band;
  • the band near 1112cm -1 is caused by the stretching vibration of CO. That is, in the spectrum of the bulk aerogel phase change composite material, no new peak appears, indicating that the phase change core material and the carrier of the phase change core material are only a physical combination, and there is no chemical interaction between the two components and can be retained The performance of the phase change core material itself.
  • the differential scanning calorimetry (DSC) chart is shown in Figure 4; the DSC test results show that the phase transition temperature of the bulk aerogel phase change composite material is 57.40/25.07°C, and the latent heat of phase change is 90.63/83.14J/g.
  • a method for preparing a bulk aerogel phase change composite material includes the following steps:
  • the prepared bulk aerogel phase change composite material has a phase change temperature of 57.40/25.07°C and a phase change latent heat of 90.63/83.14J/g.
  • Example 4 adds a block made of methyltrimethoxysilane co-precursor system
  • the aerogel phase change composite material can withstand compression deformation of about 45%.
  • the bulk aerogel phase change composite material obtained without the silane co-precursor in Example 3 which can withstand compression deformation of about 18%), Has better mechanical properties.
  • the flexibility of the skeleton is provided by the flexible molecular chain derived from the soft C-C segment, which helps it to obtain good performance in the compression test.
  • a method for preparing a bulk aerogel phase change composite material includes the following steps:
  • the prepared bulk aerogel phase change composite material has a phase change temperature of 60.30/52.10°C and a phase change latent heat of 106.38/102.31 J/g.
  • a method for preparing a bulk aerogel phase change composite material includes the following steps:
  • the DSC chart of the obtained bulk aerogel phase change composite material is shown in Figure 6; the DSC test results show that the phase change temperature is 60.13/53.13°C, and the latent heat of phase change is 133.94/132.93 J/g.
  • the embodiment of the present invention provides a bulk aerogel, a bulk aerogel phase change composite material, its preparation method and application, by adding terephthalaldehyde and organosilane monomers to the solvent; the solvothermal method obtains the condensation Glue material; dried to obtain a bridged polysilsesquioxane aerogel, that is, a bulk aerogel, the prepared bridged polysilsesquioxane aerogel has a blocky, porous structure; it can be used as a phase change
  • the carrier of the material encapsulates the phase change core material; and the amount of encapsulation of the phase change core material is large.
  • the phase change core material, terephthalaldehyde and organosilane monomers are added to the solvent; the gel material is obtained by the solvothermal method; the bulk aerogel phase change composite material is obtained by drying, and the bridge polymerization
  • the pore structure of the semisiloxane aerogel carrier material restricts the absorption of the phase change core material in its pores, which can effectively prevent the core material from leaking.

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Abstract

本发明实施例涉及纳米复合相变材料领域，具体涉及一种块体气凝胶、块体气凝胶相变复合材料、其制备方法及应用。本发明提供的块体气凝胶的制备方法，以对苯二甲醛和有机硅烷单体为原料，合成桥联聚倍半硅氧烷前驱体，经溶剂热法，不需要复杂的溶剂置换步骤，经常压干燥即可得到桥联聚倍半硅氧烷气凝胶，即块体气凝胶；制得的桥联聚倍半硅氧烷气凝胶呈块状、多孔结构，可用做相变材料的载体封装相变芯材，且对相变芯材的封装量大。利用该块体气凝胶做载体封装相变芯材得到的块体气凝胶相变复合材料，可有效解决芯材泄露、相分离和腐蚀等问题，可用于电动汽车电池系统，有效吸收电动汽车使用过程中产生的大量热量，满足冬季车内供暖需求。

Description

一种块体气凝胶、块体气凝胶相变复合材料、其制备方法及应用
交叉引用
本发明要求在中国专利局提交的、申请号为2019105010962、发明名称为“一种块体气凝胶、其制备方法及应用”的中国专利申请的优先权，该申请的全部内容通过引用结合在本发明中。本发明要求在中国专利局提交的、申请号为2019105007885、发明名称为“一种块体气凝胶相变复合材料、其制备方法及应用”的中国专利申请的优先权，该申请的全部内容通过引用结合在本发明中。
技术领域
本发明涉及纳米复合相变材料领域，具体涉及一种块体气凝胶、块体气凝胶相变复合材料、其制备方法及应用。
背景技术
随着能源短缺及环境污染等问题日益加剧，近年来，环保节能型纯电动汽车受人们广泛关注，使用越来越多。蓄电池作为电动汽车的动力来源，一方面，由于电动汽车工作原理的限制，冬季没有发动机的循环冷却液来供热，只能依靠电加热进行车内供暖，空调系统的高电能耗导致电动汽车续航能力大幅度降低；另一方面，由于蓄电池高强度放电会源源不断地产生大量的热量，产生的热量直接影响电池的性能、寿命、耐久性。因此，研究锂电池的热管理及热利用以保证电池的正常工作是十分重要的。
相变材料能够在相变过程中吸收或释放大量潜热，在能量存储方面有着重要的应用。选用一种储能密度大，质量轻，热稳定性高的相变材料用于动力电池热管理系统回收余热并进行存储，能够保证电池在正常的工作温度条件下工作，同时在需要热量的时候可以释放热量用于冬季车内供暖，以减少空调系统电能消耗维持汽车续航里程。但尚未有能够很好地满足动力电池热管理系统要求的相变材料。此外，现有相变材料的制备方法，为两步法，即先制得载体材料，再用载体吸附相变芯材，从而制得相变材料，步骤繁琐不可控。
公开于该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解，而不应当被视为承认或以任何形式暗示该信息构成已为本领域一般技 术人员所公知的现有技术。
发明内容
发明目的
为解决上述技术问题，本发明的目的在于提供一种块体气凝胶、块体气凝胶相变复合材料、其制备方法及应用。本发明提供的块体气凝胶的制备方法，以对苯二甲醛和有机硅烷单体为原料合成桥联聚倍半硅氧烷前驱体，经溶剂热法及干燥即可得到桥联聚倍半硅氧烷气凝胶，即块体气凝胶；制得的桥联聚倍半硅氧烷气凝胶呈块状、多孔结构，可用做相变材料的载体封装相变芯材，且对相变芯材的封装量大。本发明提供的块体气凝胶相变复合材料的制备方法，以所述块体气凝胶为载体材料，在制备块体气凝胶的起始阶段即加入相变芯材，气凝胶的制备和相变芯材的封装同时进行，一步即得，制备方法简单、快速。本发明提供的块体气凝胶相变复合材料的制备方法制得的块体气凝胶相变复合材料，为一种新型相变材料，具有良好的热性能及稳定性，还具有一定的隔热性能，控温范围恒定，且可有效解决芯材泄露、相分离和腐蚀等问题，实现热能储存和温度调控的一体化。本发明的制备方法制得的块体气凝胶相变复合材料可用于电动汽车电池系统，可有效吸收电动汽车使用过程中产生的大量热量，满足冬季车内供暖需求，解决空调系统高电能耗导致续航里程减少的问题。
解决方案
为实现本发明目的，本发明实施例提供了一种块体气凝胶的制备方法，所述制备方法包括：
向溶剂中加入对苯二甲醛和有机硅烷单体；溶剂热法得到凝胶材料；干燥，得到桥联聚倍半硅氧烷气凝胶，即块体气凝胶。
上述块体气凝胶的制备方法在一种可能的实现方式中，所述制备方法包括：向溶剂中加入对苯二甲醛、有机硅烷单体和硅烷共前驱体。
上述块体气凝胶的制备方法在一种可能的实现方式中，溶剂热法反应温度为100-150℃，可选地为120℃；反应时间为20-28h。
上述块体气凝胶的制备方法在一种可能的实现方式中，干燥温度为70-80℃；干燥时间为40-48h。
上述块体气凝胶的制备方法在一种可能的实现方式中，对苯二甲醛和有机硅烷单体的摩尔比为1：1.8-2.3。
上述块体气凝胶的制备方法在一种可能的实现方式中，有机硅烷单体包括：3-氨基丙基三乙氧基硅烷(CAS号为919-30-2)、3-氨基丙基三甲氧基硅烷(CAS号为13822-56-5)、(3-氨基丙基)-二乙氧基甲基硅烷(CAS号为3179-76-8)、(3-氨基丙基)二甲基乙氧基硅烷(CAS号为18306-79-1)中的一种或多种。
上述块体气凝胶的制备方法在一种可能的实现方式中，硅烷共前驱体包括甲基三甲氧基硅烷(CAS号为1185-55-3)、四乙氧基硅烷(CAS号为78-10-4)、甲基三乙氧基硅烷(CAS号为2031-67-6)、三甲氧基丙基硅烷(CAS号为1067-25-0)、甲氧基三甲基硅烷(CAS号为1825-61-2)中的一种或多种。
本发明实施例还提供了上述块体气凝胶的制备方法制得的块体气凝胶。
本发明实施例还提供了一种块体气凝胶相变复合材料的制备方法，所述制备方法包括：
向溶剂中加入相变芯材、对苯二甲醛和有机硅烷单体；溶剂热法得到凝胶材料；干燥，得到块体气凝胶相变复合材料。
其中，有机硅烷单体包括有机桥联基团和功能化的甲基硅烷。对苯二甲醛中的两个醛基基团，可与有机硅烷单体中的氨基基团反应，合成桥联聚倍半硅氧烷前驱体，经溶剂热法及干燥后，即可得到块状多孔的桥联聚倍半硅氧烷气凝胶。此外，在制备桥联聚倍半硅氧烷气凝胶时即加入相变芯材，可实现气凝胶的制备和相变芯材的封装一步完成，得到的块体气凝胶相变复合材料为封装了相变芯材的块状多孔的桥联聚倍半硅氧烷气凝胶。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，所述制备方法包括：向溶剂中加入相变芯材、对苯二甲醛、有机硅烷单体和硅烷共前驱体。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，所述制备方法包括：干燥温度高于相变芯材的相变温度。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，溶剂为乙醇。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，所述制备方法包括下述步骤：
将对苯二甲醛和相变芯材溶于乙醇，超声；然后加入有机硅烷单体，超声；再加入去离子水，超声分散，转移到反应釜内；
将反应釜置于烘箱中反应，得到凝胶材料；
将反应釜内胆取出放入烘箱中干燥，得到块体气凝胶相变复合材料；其中，干燥温度高于相变芯材的相变温度；
可选地，除有机硅烷单体外还加入硅烷共前驱体。加入去离子水的作用是促进硅烷的水解。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，各步超声时的功率为400-700W，可选地为600W；超声时间为5-25min。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，将反应釜置于烘箱中反应时，烘箱温度为100-150℃，可选地为120℃；反应时间为20-28h。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，将反应釜内胆取出放入烘箱中干燥时，干燥温度为70-80℃；干燥时间为40-48h。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，对苯二甲醛和有机硅烷单体的摩尔比为1：1.8-2.3。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，相变芯材和气凝胶载体的质量比为1-100：1-100；可选地为20-70：100；进一步可选地为50-70：100。其中，气凝胶载体指的是其余步骤均相同，但不加入相变芯材制得的桥联聚倍半硅氧烷气凝胶。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，硅烷共前驱体和有机硅烷单体的摩尔比为1-2：1；可选地为1：1或2：1。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，乙醇的加入量为5-15mL；可选地为7-10mL；进一步可选地为7.5-8mL。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，有机硅烷单体包括：3-氨基丙基三乙氧基硅烷、3-氨基丙基三甲氧基硅烷、(3-氨基丙基)-二乙氧基甲基硅烷、(3-氨基丙基)二甲基乙氧基硅烷中的一种或多种。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，相变芯材包括：多元醇类、脂肪酸类、石蜡类中的一种或多种；可选地，多元醇类包括平均分子量为600-10000的聚乙二醇、季戊四醇、新戊二醇中的一种或多种；脂肪酸类包括硬脂酸、肉豆蔻酸、棕榈酸、癸酸、月桂酸、十五烷酸、十八醇、十八酸、十八胺、十八烷中的一种或多种。
上述块体气凝胶相变复合材料的制备方法在一种可能的实现方式中，硅烷共前驱体包括甲基三甲氧基硅烷、四乙氧基硅烷、甲基三乙氧基硅烷、三甲氧基丙基硅烷、甲氧基三甲基硅烷中的一种或多种。
本发明实施例还提供了上述块体气凝胶相变复合材料的制备方法制得的块体气凝胶相变复合材料。
本发明实施例还提供了上述块体气凝胶的制备方法、块体气凝胶、块体气凝胶相变复合材料的制备方法或块体气凝胶相变复合材料在电动汽车电池系统中的应用。
上述应用在一种可能的实现方式中，所述应用包括：用于电动汽车电池系统内的余热回收以用于电动汽车冬季供暖。
有益效果
(1)本发明实施例提供的块体气凝胶的制备方法，以对苯二甲醛和有机硅烷单体为原料合成桥联聚倍半硅氧烷前驱体，经溶剂热法，不需要复杂的溶剂置换步骤，经常压干燥即可得到桥联聚倍半硅氧烷气凝胶，制得的桥联聚倍半硅氧烷气凝胶呈块状、多孔结构；可用做相变材料的载体封装相变芯材；且对相变芯材的封装量大，封装量(即负载量，指相变芯材与气凝胶载体材料的质量比)可达70％，实际应用时可根据不同需求调节负载量大小。
(2)本发明实施例中提供的块体气凝胶相变复合材料的制备方法，以桥联聚倍半硅氧烷气凝胶为载体，在制备桥联聚倍半硅氧烷气凝胶的起始阶段即加入相变芯材，可实现气凝胶的制备和相变芯材的封装一步完成，制备方法简单、快速。
利用桥联聚倍半硅氧烷气凝胶载体材料的孔道结构将相变芯材吸附限制在其孔道中，可有效阻止芯材泄露。通过调节相变芯材的种类和负载量，可制备一系列适于不同工作温度的块体气凝胶相变复合材料。
(3)本发明实施例中提供的块体气凝胶相变复合材料的制备方法，同时还可引入不同种类的硅烷共前驱体，引入的硅烷共前驱体可改善气凝胶相变复合材料的力学性能，赋予气凝胶材料柔性、疏水性等。
此外，通过改变加入的硅烷共前驱体的种类和质量，可调节载体材料桥联聚倍半硅氧烷气凝胶的孔径，从而更好的适配不同种类的相变芯材。
(4)本发明提供的制备方法制得的块体气凝胶相变复合材料，为封装了相变芯材的块状多孔的桥联聚倍半硅氧烷气凝胶，是一种新型材料，具有 良好的热性能(相变潜热高，储能高)及稳定性，且因其热导率低，其还具有一定的隔热性能，可实现隔热与热能储存和温度调控的一体化。
(5)本发明提供的制备方法制得的新型块体气凝胶相变复合材料，密度低、价格成本低，可有效吸收电动汽车使用过程时产生的大量热量，满足冬季车内供暖需求，解决空调系统高电能耗导致续航里程减少的问题。
附图说明
一个或多个实施例通过与之对应的附图中的图片进行示例性说明，这些示例性说明并不构成对实施例的限定。在这里专用的词“示例性”意为“用作例子、实施例或说明性”。这里作为“示例性”所说明的任何实施例不必解释为优于或好于其它实施例。
图1为本发明实施例3得到的块体气凝胶复合相变材料样品图。
图2为本发明实施例3得到的块体气凝胶复合相变材料扫描电子显微镜(SEM)扫描图。
图3为本发明实施例3得到的块体气凝胶复合相变材料的傅里叶红外光谱仪(FTIR)图谱。
图4为本发明实施例3得到的块体气凝胶复合相变材料的差示扫描量热(DSC)图谱。
图5为本发明实施例3和4得到的块体气凝胶复合相变材料的应力-应变曲线。
图6为本发明实施例6得到的块体气凝胶复合相变材料的DSC图谱。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合一个或多个实施例以及与之对应的附图对本发明实施例中的技术方案进行清楚、完整的示例性说明。
显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。除非另有其它明确表示，否则在整个说明书和权利要求书中，术语“包括”或其变换如“包含”或“包括有”等等将被理解为包括所陈述的组成部分，而并 未排除其它元件或其它组成部分。
这些实施例并不构成对保护范围的限定。除非另有说明，这里的任何实施例不必解释为优于或好于其它实施例。
另外，为了更好的说明本发明，在下文的实施例中给出了众多的具体细节。本领域技术人员应当理解，没有某些具体细节，本发明同样可以实施。在一些实施例中，对于本领域技术人员熟知的方法、手段、元件、通常按照常规条件以及手册中所述的条件或按照制造厂商所建议的条件的实验方法未作详细描述，以便于凸显本发明的主旨。所用的材料、试剂等，如无特殊说明，均为常规可由商业途径获得的。
以下实施例中原料均为市售产品。
实施例1
一种块体气凝胶的制备方法，包括下述步骤：
称量0.283g(0.002mol)对苯二甲醛与7.5mL乙醇混合，在35℃(指超声波清洗机水温)下超声20min；
然后向溶液中加入1mL(0.946g，0.0043mol)3-氨丙基三乙氧基硅烷，超声5min；
最后加入0.25mL去离子水，超声分散20min，转移到反应釜内；其中，超声功率均为600W；
将反应釜置于120℃的烘箱中反应24h，得到凝胶材料；
取出反应釜内胆放入烘箱中，80℃干燥48h，得到块体气凝胶。
实施例2
一种块体气凝胶的制备方法，包括下述步骤：
称量0.283g(0.002mol)对苯二甲醛与7.5mL乙醇混合，在35℃(指超声波清洗机水温)下超声20min；
然后向溶液中加入1mL(0.946g，0.0043mol)3-氨丙基三乙氧基硅烷和0.61mL(0.5795g，0.0043mol)甲基三甲氧基硅烷，超声5min；
最后加入0.25mL去离子水，超声分散20min，转移到反应釜内；其中，超声功率均为600W；
将反应釜置于120℃的烘箱中反应24h，得到凝胶材料；
取出反应釜内胆放入烘箱中，80℃干燥48h，得到块体气凝胶。
实施例3
一种块体气凝胶相变复合材料的制备方法，包括下述步骤：
称量0.283g(0.002mol)对苯二甲醛、0.75g PEG2000，与7.5mL乙醇混合，在35℃(指超声波清洗机水温)下超声20min；
然后向溶液中加入1mL(0.946g，0.0043mol)3-氨丙基三乙氧基硅烷，超声5min；
最后加入0.25mL去离子水，超声分散20min，转移到反应釜内；其中，超声功率均为600W；
将反应釜置于120℃的烘箱中反应24h，得到凝胶材料；
取出反应釜内胆放入烘箱中，80℃干燥48h，得到块体气凝胶相变复合材料；其PEG2000的负载量(PEG2000的质量/对应的块体气凝胶载体的质量)为60％。
制得的块体气凝胶相变复合材料样品如图1所示；
其扫描电子显微镜(SEM)扫描图如图2所示；由SEM扫描图可知，块体气凝胶相变复合材料保留了对应的块体气凝胶原始颗粒(均由随机初级纳米颗粒和聚集的大颗粒组成)的形貌；三维网状多孔结构由原始粗糙表面向光滑表面的演化证明相变芯材负载成功。
其傅里叶红外光谱仪(FTIR)分析结果如图3所示；其中，图中曲线“pure PEG2000”是相变芯材PEG2000的FTIR分析结果；曲线“aerogel”是实施例1制得的块体气凝胶(其制备步骤与实施例3相同，差别仅在于不负载相变芯材PEG2000)的FTIR分析结果；曲线“60％PEG2000@aerogel”是实施例3制得的相变芯材负载量为60％的块体气凝胶相变复合材料的FTIR分析结果。
FTIR分析结果显示，在对应的块体气凝胶谱图中，-OH的对称不对称拉伸振动出现在3431cm -1处；官能团-CH＝N-的拉伸振动出现在1642cm -1处；Si-O-Si的非对称拉伸、拉伸振动和弯曲振动分别与1041cm -1、785cm -1和461cm -1处的峰值对应；3-氨丙基三乙氧基硅烷上甲基和亚甲基的C-H键分别对应2931cm -1和2950cm -1处的峰。
相变芯材PEG2000的谱图中，C-O的拉伸振动和O-H的拉伸振动分别产生了1109cm -1和3444cm -1的吸收带；此外，在963cm -1和2887cm -1处可以观测到-CH 2拉伸振动的峰值。
制得的块体气凝胶相变复合材料的谱图中，3424cm -1处的一个谱带属于-OH拉伸振动2885cm -1处出现了与-CH 2对称拉伸振动相对应的吸收谱带；1112cm -1附近的条带是由C-O的拉伸振动引起的。即，在块体气凝胶相变复 合材料的光谱中，没有出现新的峰，说明相变芯材和相变芯材的载体只是物理组合，两种组分之间没有化学作用，可保留相变芯材本身的性能。
其差示扫描量热(DSC)图如图4所示；DSC测试结果显示块体气凝胶相变复合材料的相变温度为57.40/25.07℃，相变潜热为90.63/83.14J/g。
实施例4
一种块体气凝胶相变复合材料的制备方法，包括下述步骤：
称量0.283g(0.002mol)对苯二甲醛、1.125g PEG2000，与7.5mL乙醇混合，在35℃(指超声波清洗机水温)下超声20min；
然后向溶液中加入1mL(0.946g，0.0043mol)3-氨丙基三乙氧基硅烷和0.61mL(0.5795g，0.0043mol)甲基三甲氧基硅烷，超声5min；
最后加入0.25mL去离子水，超声分散20min，转移到反应釜内；其中，超声功率均为600W；
将反应釜置于120℃的烘箱中反应24h，得到凝胶材料；
取出反应釜内胆放入烘箱中，80℃干燥48h，得到块体气凝胶相变复合材料；其PEG2000的负载量为60％。
制得的块体气凝胶相变复合材料，其相变温度为57.40/25.07℃，相变潜热为90.63/83.14J/g。
实施例3和4制得的块体气凝胶相变复合材料的应力-应变曲线分别见图5；由图5可知，实施例4加入了甲基三甲氧基硅烷共前驱体制得的块体气凝胶相变复合材料，可承受约45％的压缩变形，较于实施例3不加硅烷共前驱体得到的块体气凝胶相变复合材料(可承受约18％的压缩变形)，具有更好的机械性能。实施例4的相变复合材料，其骨架的柔韧性是由软C-C段衍生的柔性分子链提供的，这有助于其在压缩试验中获得良好的性能。
实施例5
一种块体气凝胶相变复合材料的制备方法，包括下述步骤：
称量0.283g(0.002mol)对苯二甲醛、0.75g十八醇，与7.5mL乙醇混合，在35℃(指超声波清洗机水温)下超声20min；
然后向溶液中加入1mL(0.946g，0.0043mol)3-氨丙基三乙氧基硅烷，超声5min；
最后加入0.25mL去离子水，超声分散20min，转移到反应釜内；其中，超声功率均为600W；
将反应釜置于120℃的烘箱中反应24h，得到凝胶材料；
取出反应釜内胆放入烘箱中，80℃干燥48h，得到块体气凝胶相变复合材料；其十八醇的负载量为60％。
制得的块体气凝胶相变复合材料，其相变温度是60.30/52.10℃，相变潜热是106.38/102.31 J/g。
实施例6
一种块体气凝胶相变复合材料的制备方法，包括下述步骤：
称量0.283g(0.002mol)对苯二甲醛、1.125g十八醇，与7.5mL乙醇混合，在35℃(指超声波清洗机水温)下超声20min；
然后向溶液中加入1mL(0.946g，0.0043mol)3-氨丙基三乙氧基硅烷和0.61mL(0.5795g，0.0043mol)甲基三甲氧基硅烷，超声5min；其中，超声功率均为600W；
最后加入0.25mL去离子水，超声分散20min，转移到反应釜内；
将反应釜置于120℃的烘箱中反应24h，得到凝胶材料；
取出反应釜内胆放入烘箱中，80℃干燥48h，得到块体气凝胶相变复合材料；其十八醇的负载量为60％。
制得的上述块体气凝胶相变复合材料的DSC图如图6所示；DSC测试结果显示，其相变温度是60.13/53.13℃，相变潜热是133.94/132.93 J/g。
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
工业实用性
本发明实施例提供的一种块体气凝胶、块体气凝胶相变复合材料、其制备方法及应用，通过向溶剂中加入对苯二甲醛和有机硅烷单体；溶剂热法得到凝胶材料；干燥，得到桥联聚倍半硅氧烷气凝胶，即块体气凝胶，制得的桥联聚倍半硅氧烷气凝胶呈块状、多孔结构；可用做相变材料的载体封装相变芯材；且对相变芯材的封装量大。本发明实施例通过向溶剂中加入相变芯材、对苯二甲醛和有机硅烷单体；溶剂热法得到凝胶材料；干燥，得到块体气凝胶相变复合材料，利用桥联聚倍半硅氧烷气凝胶载体材料的孔道结构将相变芯材吸附限制在其孔道中，可有效阻止芯材泄露。

Claims (14)

  1. 一种块体气凝胶的制备方法，其特征在于，所述制备方法包括：
    向溶剂中加入对苯二甲醛和有机硅烷单体；溶剂热法得到凝胶材料；干燥，得到桥联聚倍半硅氧烷气凝胶，即块体气凝胶。
  2. 根据权利要求1所述的块体气凝胶的制备方法，其特征在于，所述制备方法包括：向溶剂中加入对苯二甲醛、有机硅烷单体和硅烷共前驱体。
  3. 根据权利要求2所述的块体气凝胶的制备方法，其特征在于，硅烷共前驱体包括甲基三甲氧基硅烷、四乙氧基硅烷、甲基三乙氧基硅烷、三甲氧基丙基硅烷、甲氧基三甲基硅烷中的一种或多种。
  4. 根据权利要求1所述的块体气凝胶的制备方法，其特征在于，溶剂热法反应温度为100-150℃；反应时间为20-28h；
    和/或，干燥温度为70-80℃；干燥时间为40-48h；
    和/或，对苯二甲醛和有机硅烷单体的摩尔比为1：1.8-2.3；
    和/或，有机硅烷单体包括：3-氨基丙基三乙氧基硅烷、3-氨基丙基三甲氧基硅烷、(3-氨基丙基)-二乙氧基甲基硅烷、(3-氨基丙基)二甲基乙氧基硅烷中的一种或多种。
  5. 权利要求1-4任一项所述的块体气凝胶的制备方法制得的块体气凝胶。
  6. 一种块体气凝胶相变复合材料的制备方法，其特征在于，所述制备方法包括：
    向溶剂中加入相变芯材、对苯二甲醛和有机硅烷单体；溶剂热法得到凝胶材料；干燥，得到块体气凝胶相变复合材料。
  7. 根据权利要求6所述的块体气凝胶相变复合材料的制备方法，其特征在于，向溶剂中加入相变芯材、对苯二甲醛、有机硅烷单体和硅烷共前驱体。
  8. 根据权利要求7所述的块体气凝胶相变复合材料的制备方法，其特征在于，硅烷共前驱体和有机硅烷单体的摩尔比为1-2：1；
    和/或，硅烷共前驱体包括甲基三甲氧基硅烷、四乙氧基硅烷、甲基三乙氧基硅烷、三甲氧基丙基硅烷、甲氧基三甲基硅烷中的一种或多种。
  9. 根据权利要求6所述的块体气凝胶相变复合材料的制备方法，其特征在于，相变芯材和气凝胶载体的质量比为1-100：1-100；可选地为20-70：100；进一步可选地为50-70：100；
    和/或，干燥温度高于相变芯材的相变温度；
    和/或，溶剂为乙醇；
    和/或，对苯二甲醛和有机硅烷单体的摩尔比为1：1.8-2.3；
    和/或，有机硅烷单体包括：3-氨基丙基三乙氧基硅烷、3-氨基丙基三甲氧基硅烷、(3-氨基丙基)-二乙氧基甲基硅烷、(3-氨基丙基)二甲基乙氧基硅烷中的一种或多种；
    和/或，相变芯材包括：多元醇类、脂肪酸类、石蜡类中的一种或多种；多元醇类包括平均分子量600-10000的聚乙二醇、季戊四醇、新戊二醇中的一种或多种；脂肪酸类包括硬脂酸、肉豆蔻酸、棕榈酸、癸酸、月桂酸、十五烷酸、十八醇、十八酸、十八胺、十八烷中的一种或多种。
  10. 根据权利要求6所述的块体气凝胶相变复合材料的制备方法，其特征在于，所述制备方法包括下述步骤：
    将对苯二甲醛和相变芯材溶于乙醇，超声；然后加入有机硅烷单体，超声；再加入去离子水，超声分散，转移到反应釜内；
    将反应釜置于烘箱中反应，得到凝胶材料；
    将反应釜内胆取出放入烘箱中干燥，得到块体气凝胶相变复合材料；其中，干燥温度高于相变芯材的相变温度；
    可选地，除有机硅烷单体外还加入硅烷共前驱体。
  11. 根据权利要求10所述的块体气凝胶相变复合材料的制备方法，其特征在于，各步超声时的功率为400-700W；超声时间为5-25min；
    和/或，将反应釜置于烘箱中反应时，烘箱温度为100-150℃；反应时间为20-28h；
    和/或，将反应釜内胆取出放入烘箱中干燥时，干燥温度为70-80℃；干燥时间为40-48h。
  12. 权利要求6-11任一项所述的块体气凝胶相变复合材料的制备方法制得的块体气凝胶相变复合材料。
  13. 权利要求1-4任一项所述的块体气凝胶的制备方法或权利要求5所述的块体气凝胶或权利要求6-11任一项所述的块体气凝胶相变复合材料的制备方法或权利要求12所述的块体气凝胶相变复合材料在电动汽车电池系统中的应用。
  14. 根据权利要求13所述的应用，其特征在于：所述应用包括：用于电动汽车电池系统内的余热回收以用于电动汽车冬季供暖。
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