CN105399889B - 一种相变储能材料的杂化壁材纳米胶囊及其制备方法 - Google Patents
一种相变储能材料的杂化壁材纳米胶囊及其制备方法 Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/34—Monomers containing two or more unsaturated aliphatic radicals
- C08F212/36—Divinylbenzene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
Abstract
本发明公开了一种相变储能材料的杂化壁材纳米胶囊及其制备方法,具体是将相变储能材料、烷氧基硅烷类化合物、乙烯基单体和引发剂混合形成油相,加入水相和乳化剂,乳化后再超声均化,形成细乳液,通入氮气除氧,并加入碱性催化剂,密闭或持续通氮气保护条件下搅拌反应,得到相变储能材料纳米胶囊与水相的混合物;将所述混合物过滤,去离子水洗涤,干燥,即得粉末状的产品。本发明的产品形貌规则,粒径小于1μm,比表面积大,热量存储/释放效率高,相变焓和热稳定性高,并可以耐受大于1000次芯材熔融‑结晶过程;本发明的产品可与多种无机材料和有机聚合物复合制成调温复合材料,相容性好,对力学性能的影响小。
Description
技术领域
本发明的实施方式涉及相变储能材料的胶囊,更具体地,本发明的实施方式涉及一种相变储能材料的杂化壁材纳米胶囊及其制备方法。
背景技术
由于传统化石能源的稀缺和不可再生性、世界人口的不断增加、和温室气体排放量的持续增长,高效利用能源和发展新的能源储存技术变得日益重要。近几十年来,相变储能材料(PCMs)受到了很大关注,其具有储热密度大和接近等温储热的优势,可以作为清洁的可持续能源储存材料。PCMs大多通过固-液相变过程进行热能的储存和释放,为防止其在熔融状态下的泄露,提高热能储存/释放效率,并控制其在相变过程中的体积变化,微/纳米胶囊化PCMs得到了很大发展,并广泛用于太阳能储存、制冷系统、节能建筑和智能织物等许多领域。其中,微胶囊化相变材料(MicroPCMs)的尺寸在1~1000μm范围,而纳米胶囊化相变材料(NanoPCMs)的尺寸通常在几十纳米到1μm范围。
微/纳米胶囊化PCMs通常由芯材(即PCMs)和壁材两部分组成,并形成核-壳结构。传统上,各种有机聚合物材料被用于胶囊壁材,例如三聚氰胺-甲醛树脂、脲醛树脂、聚脲、聚苯乙烯(PS)和聚甲基丙烯酸甲酯(PMMA)等。有机壁材的种类丰富,具有很好的结构弹性,有利于承受PCMs在使用过程中体积的反复变化,但存在热导率低、热和化学稳定性较差、易燃、释放有害气体(甲醛等)等不足。近年来,无机材料如二氧化硅(SiO2)、勃姆石、碳酸钙、二氧化钛等作为胶囊壁材引起了研究者的很大兴趣和关注。与有机聚合物壁材相比,无机壁材通常具有较高的热导率、优异的热/化学稳定性、不燃、不释放有害气体等优势,但也存在一些明显的局限性,如脆性较大、力学强度差、常常形成多孔结构等。
有机-无机杂化材料使有机和无机成分在分子水平或纳米尺度上复合,作为微/纳米胶囊化PCMs的壁材,可以赋予其优异的力学性能、耐久性和包覆率。目前仅有少量文献报道了以有机-无机杂化材料作为壁材的PCMs胶囊及其制备方法,其粒径均在微米量级。Chang等(J.Appl.Polym.Sci.2009,112,1850)采用自由基聚合与溶胶-凝胶(sol-gel)反应结合的方法,制备了以PMMA-SiO2杂化材料为壁材,以正十八烷为芯材的MicroPCMs,粒径约为10μm,SiO2(5wt%)的引入提高了PCMs的包覆率。Li等(Energy.2014,70,298)以γ-甲基丙烯酰氧基丙基三甲氧基硅烷(MPS)和乙烯基三甲氧基硅烷(VTMS)作为原料,通过自由基聚合与sol-gel反应结合的方法,获得了以有机-无机杂化材料作为壁材,以正十八烷为芯材的MicroPCMs,其具有较高的相变焓和良好的防渗透性。Yin等(Energy.2014,64,575)利用皮克林(Pickering)乳液聚合法,以SiO2纳米粒子作为乳化剂,制备了以PS-SiO2杂化材料为壁材、以正十二醇为芯材的MicroPCMs,粒径约为60μm,并获得了较高的包覆率和热循环耐久性。Zhang等(J.Mater.Chem.A.2014,2,5304)利用疏水改性氧化石墨烯(GO)作为稳定剂,合成了以PS-GO杂化材料为壁材,以正十六烷为芯材的MicroPCMs,粒径为20~30μm。与MicroPCMs相比,NanoPCMs具有更小的尺寸和更大的比表面积,因此热能储存和释放的效率更高。并且,当用于潜热功能流体时,NanoPCMs在导热介质的输送过程中不易破裂。然而,目前尚没有以有机-无机杂化材料作为壁材的NanoPCMs的公开报道。
发明内容
基于上述现有技术的缺陷,本发明希望开发一种相变储能材料的杂化壁材纳米胶囊的制备方法,及其对应制得的形貌规则、相变焓和热稳定性高的相变储能材料纳米胶囊。
本发明通过以下技术方案达到上述目的:
一种相变储能材料的杂化壁材纳米胶囊的制备方法,它包括以下步骤:
(1)将以质量计30%~70%的相变储能材料、10%~60%的烷氧基硅烷类化合物、5%~60%的乙烯基单体和0~2%的引发剂在反应釜中混合形成油相;
(2)将以质量计20%~100%的水和0~80%的乙醇配制成水相,并按水相和油相质量比2~50:1将水相加入所述油相中,然后加入水相质量0.2%~5%的乳化剂,搅拌或剪切力作用下乳化,接着超声均化,使所述油相和水相均匀混合形成细乳液,所述细乳液中油相分散于水相中形成纳米级的液滴;
(3)向所述细乳液中通入氮气除氧,并加入水相质量0.2%~5%的碱性催化剂,将反应釜密闭或持续通氮气保护,20~80℃搅拌反应4~8h,得到相变储能材料纳米胶囊与水相的混合物;
(4)将所述混合物过滤得到纳米胶囊,去离子水洗涤,干燥,即得粉末状的相变储能材料的杂化壁材纳米胶囊。
通过上述技术方案得到的相变储能材料的纳米胶囊可以与水或其它导热介质混合,制成悬浮液或乳液,作为热交换流体使用;也可与水泥、石膏或各种高分子材料复合,制成储热调温复合材料。
优选的,上述相变储能材料的杂化壁材纳米胶囊的制备方法中,所述相变储能材料占油相总质量的40%~60%,烷氧基硅烷类化合物占油相总质量的30%~50%,乙烯基单体占油相总质量的20%~30%,引发剂占油相总质量的0.2%~1%,水相中水的质量百分含量为60%~80%,乙醇的质量百分含量为20%~40%,水相与油相的质量比为5:1~20:1,碱性催化剂的用量为水相质量的0.4~3%。
上述相变储能材料的杂化壁材纳米胶囊的制备方法中,所述相变储能材料为石蜡、C12-28的正构烷烃、C8-18的脂肪醇、C8-18的脂肪酸及其酯中的一种或多种;所述石蜡的熔点在20~70℃,它在步骤(3)的反应温度下能够熔化。
进一步的技术方案是:所述相变储能材料为正十六烷、正十八烷、正二十烷、月桂酸、棕榈酸、硬脂酸、硬脂酸正丁酯中的一种或多种。
上述相变储能材料的杂化壁材纳米胶囊的制备方法中,所述烷氧基硅烷类化合物为正硅酸乙酯(TEOS)、甲基三甲氧基硅烷(MTMS)、γ-甲基丙烯酰氧基丙基三甲氧基硅烷(MPS)、γ-氨基丙基三甲氧基硅烷(APS)、乙烯基三甲氧基硅烷(VTMS)中的一种或多种。
上述相变储能材料的杂化壁材纳米胶囊的制备方法中,所述乙烯基单体为苯乙烯、甲基丙烯酸甲酯、丙烯酸丁酯、二乙烯基苯、双(甲基丙烯酸)乙二醇酯、甲基丙烯酸烯丙酯中的一种或多种。
上述相变储能材料的杂化壁材纳米胶囊的制备方法中,所述引发剂为偶氮二异丁腈(AIBN)、过氧化苯甲酰、叔丁基过氧化氢中的一种或多种。
上述相变储能材料的杂化壁材纳米胶囊的制备方法中,所述乳化剂为十六烷基三甲基溴化铵(CTAB)、曲拉通(TX-100)、十二烷基硫酸钠(SDS)、聚苯乙烯-马来酸酐钠盐中的一种或多种。
上述相变储能材料的杂化壁材纳米胶囊的制备方法中,所述碱性催化剂为氢氧化钠、乙二胺、三乙胺或三甲胺的水溶液以及氨水中的一种或多种。
进一步的技术方案是:所述碱性催化剂是浓度为25wt%的氨水或5wt%的氢氧化钠水溶液。
上述相变储能材料的杂化壁材纳米胶囊的制备方法中,所述干燥的条件为冷冻干燥或在50℃的真空烘箱中干燥24h。
本发明进一步公开了一种根据上述制备方法制备得到的相变储能材料的杂化壁材纳米胶囊,该纳米胶囊由有机-无机杂化材料作为壁材包覆由相变储能材料形成的胶囊核,其粒径小于1μm。
下面对本发明的技术方案进行进一步的说明。
本发明使用水和乙醇的混合溶剂作为细乳液的水相,有利于提高纳米胶囊的形貌规整性。
在碱性催化剂作用下,烷氧基硅烷类化合物在水相/油相界面处发生水解和缩合反应,生成无机的二氧化硅成分。同时,引发剂受热分解产生自由基,引发乙烯基类单体聚合,生成有机聚合物,并与油相发生相分离。无机的二氧化硅与有机聚合物在水相/油相界面处形成分子或纳米尺度上的有机-无机杂化材料。相变储能材料位于液滴中心,形成胶囊核,并被有机-无机杂化材料所包覆。
本发明中,由于反应过程中油相体积减小,在胶囊内外产生压力差,且有机-无机杂化材料壁材具有一定柔性,胶囊可能发生从球形到碗状的转变。与球形形貌相比,碗状形貌具有更大的比表面积,有利于提高相变储能材料的热能储存/释放效率。
本发明中有机-无机杂化材料包覆相变储能材料纳米胶囊的制备采用一锅法,所有反应过程均在同一反应容器中完成,制备方法简便易行。
与现有技术相比,本发明的有益效果至少包括以下几点:
(1)制备方法简便,产率高,便于大批量制备;
(2)制备方法适于制得多种不同壁材组成的相变储能材料的纳米胶囊;制备方法适于制得包覆多种不同类型的相变储能材料的纳米胶囊;
(3)制备得到的有机-无机杂化材料包覆相变储能材料纳米胶囊的形貌规则,粒径小于1μm,比表面积大,热量存储/释放效率高;制备得到的相变储能材料的纳米胶囊相变焓和热稳定性高,并可以耐受大于1000次芯材熔融-结晶过程;制备得到的相变储能材料的纳米胶囊可与多种无机材料和有机聚合物复合制成调温复合材料,相容性好,对力学性能的影响小。
(4)本发明所制备的有机-无机杂化材料包覆相变储能材料纳米胶囊应用范围广,可以用于智能调温织物、建筑节能、电子电器控温、工业制冷系统等领域。
附图说明
图1为本发明的相变储能材料的杂化壁材纳米胶囊的扫描电子显微镜(SEM)照片。
图2为本发明的相变储能材料的杂化壁材纳米胶囊的透射电子显微镜(TEM)照片。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
在100mL三口瓶中,加入1.0g正十八烷、0.75mL TEOS、0.375mL MPS、0.375mL苯乙烯、0.015g AIBN,混合形成油相。其后,依次向三口瓶内加入28.5mL水,14.2mL乙醇,水和乙醇混溶后作为水相。其后再向三口瓶内加入0.246g CTAB,在35℃下磁力搅拌30min,转速为1500r/min。然后立即使用超声清洗器(KQ-400KDB型,100%振幅)在35℃下超声10min,形成稳定的细乳液。向三口瓶内通氮气30min,之后加入质量浓度为25wt%的氨水1.04mL。持续通氮气保护,将三口瓶放入80℃油浴中,磁力搅拌4h,搅拌速率为300r/min。在此过程中,TEOS和MPS发生水解-缩合反应,MPS和苯乙烯发生自由基聚合反应,在油相/水相界面处形成有机-无机杂化材料壁材。将反应后的混合液冷却至室温,进行过滤,并用去离子水对其进行多次洗涤,之后冷冻干燥,得到白色粉末状纳米胶囊产物,其电镜图如图1和图2所示。所得胶囊为碗状,具有明确的核壳结构,平均粒径为420nm,熔融温度为26.6℃,熔融焓为110J/g。
实施例2
在1000mL烧杯中,加入10g正十八烷、7.5mL TEOS、3.75mL MPS、3.75mL苯乙烯、0.15g AIBN,混溶后形成油相。其后,依次向烧杯内加入285mL水,142mL乙醇,水和乙醇混溶后作为水相。其后再向烧杯内加入2.46g CTAB,在35℃下高速剪切(Ultra Turrax T25型,10000r/min)乳化2min。然后立即使用超声器(VCX-750型,40%振幅)在35℃下超声10min,形成稳定的细乳液。将细乳液倾入500mL三口瓶,向内通氮气30min,之后加入质量浓度为25wt%的氨水10.4mL。在三口瓶中持续通氮气保护,并放入80℃油浴中,磁力搅拌4小时,搅拌速率为300r/min。在此过程中,TEOS和MPS发生水解-缩合反应,MPS和苯乙烯发生自由基聚合反应,在油相/水相界面处形成有机-无机杂化壁材。将反应后的混合液冷却至室温,进行过滤,并用去离子水进行多次洗涤,之后冷冻干燥,得到白色粉末状纳米胶囊产物。所得胶囊为碗状,具有明确的核壳结构,平均粒径为410nm,熔融温度为26.6℃,熔融焓为115J/g。
实施例3
在1000mL烧杯中,加入10g硬脂酸正丁酯、10mL乙烯基三甲氧基硅烷、5mL甲基丙烯酸甲酯、0.15g叔丁基过氧化氢,混溶后形成油相。其后,依次向烧杯内加入320mL水,107mL乙醇,水和乙醇混溶后作为水相。其后再向烧杯内加入2.00g十二烷基硫酸钠,在35℃下高速剪切(Ultra Turrax T25型,10000r/min)乳化2min。然后立即使用超声器(VCX-750型,40%振幅)在35℃下超声10min,形成稳定的细乳液。将细乳液倾入500mL三口瓶,向内通氮气30min,之后加入质量浓度为5wt%的氢氧化钠溶液2.0mL。在三口瓶中持续通氮气保护,并放入80℃油浴中,磁力搅拌3小时,搅拌速率为300r/min。将反应后的混合液冷却至室温,进行过滤,并用去离子水进行多次洗涤,之后在50℃的真空烘箱中干燥24h,得到白色粉末状纳米胶囊产物。
实施例4
在100mL三口瓶中,加入1.0g棕榈酸、0.75mL TEOS、0.375mL APS、0.375mL二乙烯基苯、0.015g过氧化苯甲酰,混合形成油相。其后,向三口瓶内加入42.7mL水,0.427g曲拉通,在65℃下磁力搅拌15min,转速为1500r/min。然后立即使用超声清洗器(KQ-400KDB型,100%振幅)在35℃下超声5min,形成稳定的细乳液。向三口瓶内通氮气30min,之后加入质量浓度为25wt%的氨水0.26mL。持续通氮气保护,将三口瓶放入80℃油浴中,磁力搅拌6h,搅拌速率为300r/min。将反应后的混合液冷却至室温,进行过滤,并用去离子水对其进行多次洗涤,之后冷冻干燥,得到白色粉末状纳米胶囊产物。
尽管这里参照本发明的解释性实施例对本发明进行了描述,但是,应该理解,本领域技术人员可以设计出很多其他的修改和实施方式,这些修改和实施方式将落在本申请公开的原则范围和精神之内。更具体地说,在本申请公开的范围内,可以对主题组合布局的组成部件和/或布局进行多种变型和改进。除了对组成部件和/或布局进行的变型和改进外,对于本领域技术人员来说,其他的用途也将是明显的。
Claims (6)
1.一种相变储能材料的杂化壁材纳米胶囊的制备方法,其特征在于它包括以下步骤:
(1)将以质量计30%~70%的相变储能材料、10%~60%的烷氧基硅烷类化合物、5%~60%的乙烯基单体和0~2%的引发剂在反应釜中混合形成油相;所述相变储能材料为正十八烷,所述烷氧基硅烷类化合物为正硅酸乙酯和γ-甲基丙烯酰氧基丙基三甲氧基硅烷的混合物,所述乙烯基单体为苯乙烯;
(2)将以质量计20%~100%的水和0~80%的乙醇配制成水相,并按水相和油相质量比2~50:1将水相加入所述油相中,然后加入水相质量0.2%~5%的乳化剂,搅拌或剪切力作用下乳化,接着超声均化,使所述油相和水相均匀混合形成细乳液,所述细乳液中油相分散于水相中形成纳米级的液滴;
(3)向所述细乳液中通入氮气除氧,并加入水相质量0.2%~5%的碱性催化剂,将反应釜密闭或持续通氮气保护,20~80℃搅拌反应4~8h,得到相变储能材料纳米胶囊与水相的混合物;
(4)将所述混合物过滤得到纳米胶囊,去离子水洗涤,干燥,即得粉末状的相变储能材料的杂化壁材纳米胶囊。
2.根据权利要求1所述的相变储能材料的杂化壁材纳米胶囊的制备方法,其特征在于所述引发剂为偶氮二异丁腈、过氧化苯甲酰、叔丁基过氧化氢中的一种或多种。
3.根据权利要求1所述的相变储能材料的杂化壁材纳米胶囊的制备方法,其特征在于所述乳化剂为十六烷基三甲基溴化铵、曲拉通、十二烷基硫酸钠、聚苯乙烯-马来酸酐钠盐中的一种或多种。
4.根据权利要求1所述的相变储能材料的杂化壁材纳米胶囊的制备方法,其特征在于所述碱性催化剂为氢氧化钠、乙二胺、三乙胺或三甲胺的水溶液以及氨水中的一种或多种。
5.根据权利要求4所述的相变储能材料的杂化壁材纳米胶囊的制备方法,其特征在于所述碱性催化剂是浓度为25wt%的氨水或5wt%的氢氧化钠水溶液。
6.采用权利要求1~5任意一项所述的制备方法得到的相变储能材料的杂化壁材纳米胶囊。
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