CN105820540B - 一种有机阻燃定形相变储能材料及其制备方法 - Google Patents
一种有机阻燃定形相变储能材料及其制备方法 Download PDFInfo
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- CN105820540B CN105820540B CN201610198516.0A CN201610198516A CN105820540B CN 105820540 B CN105820540 B CN 105820540B CN 201610198516 A CN201610198516 A CN 201610198516A CN 105820540 B CN105820540 B CN 105820540B
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
一种有机阻燃定形相变储能材料及其制备方法,其属于新材料技术领域。该材料通过聚乙二醇与含有双官能团化合物反应,得到含双官能团中间体化合物;该中间体化合物再与反应型阻燃剂反应,将反应型阻燃剂引入到高分子骨架,得到有机高分子定形相变支撑材料,再通过物理添加的方式加入添加型阻燃剂,最后得到有机阻燃定形相变储能材料。其中有机高分子定形相变支撑材料占70~95wt%;添加型阻燃剂占5%~30%。该阻燃储热材料相变温度可调,形状稳定,阻燃性能好。该材料可用于特殊环境下热能的存储。该材料合成工艺简单,应用方便,具有广阔的应用前景。
Description
技术领域
本发明涉及一种有机阻燃定形相变储能材料及其制备方法,其属于新材料技术领域。
背景技术
近年来,能源问题一直是很热门的话题。传统能源消耗迅速,寻找传统能源的替代品成为了人们亟需解决的问题。太阳能、风能和地热能等清洁可再生能源成为了最合适的新能源,可是这些能源都存在间歇性和波动性的缺点,不能持续地、稳定地提供能量,这就需要相变储能材料(PCM)来实现稳定供能。
相变储能材料通过物理相转变(固-液,液-气等),吸收或者释放大量热量,实现能量存储与利用,是提高热能利用效率的有效方式之一,具有储能密度大,储能能力强的优点,能有效缓解能量供应上空间与时间失衡的冲突。
但是相变材料也存在着一定的问题,如大多相变材料易燃烧,易泄漏,在实际应用中有很大的限制。
为提高相变材料的阻燃性能,相关科研工作者利用吸收、包覆或涂抹阻燃剂等途径获得了具有阻燃效果的相变材料,Salyer I等人用石膏板吸收了PCM来研究相变材料的阻燃方法,一种方法是在石膏板表面形成不易燃表层,如铝箔或硬质的聚氯乙烯膜;或者使石膏板吸收液体阻燃剂取代部分相变材料以达到阻燃效果;还有一种办法是引入卤素离子,用溴化十六烷和十八烷作相变材料,与石膏板中的三氧化二锑协同阻燃,可以使石膏板具有自熄性;或者直接在石膏板表面涂上阻燃剂[SALYER I,SIRCAR A.Phase changematerials for heating and cooling of residential buildings and otherapplication[C].Proceedings of 25th Intersociety Energy Conversion EngineeringConference,Reno,Nevada,1990.]。胡源等申请了一种相变材料的阻燃方法的专利,将石蜡,阻燃剂,金属粉和聚乙烯混合后熔融挤出,得到膨胀型阻燃剂、石蜡和金属粉末均匀地分散在高密度聚乙烯中的具有空间网状结构的阻燃定形相变材料。其中使用的阻燃剂是膨胀型阻燃剂,它和金属粉末协同阻燃,从而大大减少了阻燃剂添加量,使得相变材料的热焓值损失少,阻燃效果好,能够投入实际使用[胡源,张平,宋磊.一种阻燃定形相变材料及其制备方法:中国,200810196742.0[P].2009,04,01.]。
将聚乙二醇和反应型阻燃剂引入高分子骨架,并物理添加阻燃剂,所得相变材料具有优异的形状稳定特性,较好的相变性能的同时还可以具有一定的阻燃效果。
发明内容
为解决现有技术中存在的问题,本发明提供一类新的相变温度易于调节、具有一定阻燃效果的有机阻燃定形相变储能材料,此种材料将聚乙二醇和反应型阻燃剂引入高分子骨架,并物理添加阻燃剂,得到相变温度可调,形状稳定,阻燃性能好的的新型阻燃储热材料,可用于特殊环境下热能的存储。此类材料合成工艺简单,应用方便,具有广阔的应用前景。
一种有机阻燃定形相变储能材料,其特征在于:所述有机阻燃定形相变储能材料按质量百分比,由下述组分组成:
有机高分子定形相变支撑材料:70~95wt%;添加型阻燃剂:5%~30%。
本发明所述有机阻燃定形相变储能材料将支撑材料及阻燃剂复合而成,其中,所述有机高分子定形相变支撑材料是以聚醚为软段、芳环为硬段的多嵌段型高分子相变材料。
本发明优选所述有机阻燃定形相变储能材料按质量百分比,由下述组分组成:
有机高分子定形相变支撑材料:80~90%;添加型阻燃剂:10%~20%。
所述添加型阻燃剂为四溴双酚-A,十溴二苯乙烷,磷酸三(2,3-二氯丙基)酯,聚磷酸铵,磷酸三苯酯,十溴二苯醚,磷酸三(β一氯乙基)酯,磷酸三(β-氯丙基)酯中的1~2种。
有机高分子定形相变支撑材料的结构通式如下:
其中,连接基A的结构为或
或
V1为Cl、F、NHCH3或NHC4H9;V2为H或CH3;m=10~10000的整数;n=10~1000的整数。
一种有机阻燃定形相变储能材料的制备方法,包括下述工艺步骤:搅拌条件下,将添加型阻燃剂和有机高分子定形相变支撑材料于溶剂中按比例混合0.5~2h,蒸发溶剂,真空干燥,即得。
上述技术方案中,所述溶剂优选为四氢呋喃、二氧六环、石油醚、丙酮、丁酮、氯仿、二氯甲烷、四氯化碳、二硫化碳、DMF、DMSO、苯、甲苯、二甲苯、硝基苯、氯苯、环己烷或正己烷中的1~3种。
上述技术方案中,所述有机高分子定形相变支撑材料优选按下述方法制得:
(1)将反应型阻燃剂与如下式所述的聚乙二醇在80℃条件下真空干燥48h,其中,所述反应型阻燃剂为四溴双酚-A阻燃剂。
其中m=10~10000的整数。
(2)将聚乙二醇与含有双官能团的化合物按摩尔比1:2溶于溶剂中,并加入适量催化剂,在N2环境中将上述原料置于三口瓶中,在40~80℃下搅拌反应2~10h,得到含有双官能团的中间体化合物的溶液。
其中,所述含有双官能团的化合物为含有环氧、三嗪或异氰酸酯结构的化合物;所述催化剂与聚乙二醇的质量比为1:80~150;所述溶剂与聚乙二醇的质量比为5~10:1;所述溶剂为四氢呋喃、二氧六环、石油醚、丙酮、丁酮、氯仿、二氯甲烷、四氯化碳、二硫化碳、DMF、DMSO、苯、甲苯、二甲苯、硝基苯、氯苯、环己烷或正己烷中的1~3种;
(3)按反应型阻燃剂与步骤(2)所得中间体化合物摩尔比为1:1向三口瓶中加入反应型阻燃剂,补加与步骤二等量的催化剂,恒温120℃反应2~12h,得有机高分子定形相变支撑材料。
上述步骤(2)所述含有环氧、三嗪或异氰酸酯结构的化合物优选为含异氰酸酯基的化合物,其中,异氰酸酯官能团通过酯键与聚醚相连,此时所述催化剂优选为二月桂酸二丁基锡。
上述步骤(2)所述含有环氧、三嗪或异氰酸酯结构的化合物优选含三嗪基的化合物,其中,三嗪官能团通过醚键与聚醚相连。此时所述催化剂优选为三乙胺或吡啶。
上述步骤(2)所述含有环氧、三嗪或异氰酸酯结构的化合物优选含环氧基的化合物,其中,环氧官能团通过醚键与聚醚相连。此时所述催化剂优选为氢氧化钠或氢氧化钾。
本发明的有益效果为:该材料通过聚乙二醇与含有双官能团化合物反应,得到含双官能团中间体化合物;该中间体化合物再与反应型阻燃剂反应,将反应型阻燃剂引入到高分子骨架,再通过物理添加的方式加入添加型阻燃剂,最后得到新的相变储能材料。其中有机高分子定形相变支撑材料占70~95wt%;添加型阻燃剂占5%~30%。该新型阻燃储热材料相变温度可调,形状稳定,阻燃性能好。该材料可用于特殊环境下热能的存储。该材料合成工艺简单,应用方便,具有广阔的应用前景。
附图说明
图1为实施例1中材料的红外谱图;
其中:a、聚乙二醇10000,b、四溴双酚-A,c、聚氨酯,d、聚氨酯/四溴双酚-A。
图2为实施例1中材料的XRD曲线。
图3为实施例1中材料的DSC曲线。
图4为实施例1中材料在30℃,70℃及95℃条件下加热15min后的定形性能。
图5为实施例1中材料的TG及DTG曲线。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。
下述实施例中所述试验方法,如无特殊说明,均为常规方法;所述试剂和材料,如无特殊说明,均可从商业途径获得。
具体实施方式
(1)将聚乙二醇及反应型阻燃剂在80℃条件下真空干燥48h,反应型阻燃剂为四溴双酚-A(其结构如下表1#所示)的阻燃剂。
(2)将聚乙二醇与含有双官能团的化合物按摩尔比1:2溶于溶剂中,并加入催化剂二月桂酸二丁基锡,催化剂与聚乙二醇的质量比为1:80~150;溶剂与聚乙二醇的质量比为5~10:1;在N2环境中将上述原料置于三口瓶中,在40~80℃下搅拌反应2~10h,得含有双官能团的中间体化合物的溶液。其中,含有双官能团的中间体化合物为含有环氧基的中间体化合物(其部分结构如下表2#、3#所示)、含有三嗪基的中间体化合物(其部分结构如下表4#、5#所示)和含有异氰酸酯基的中间体化合物(其部分结构如下表6#、7#、8#、9#、10#、11#、12#、13#所示)。溶剂为四氢呋喃、二氧六环、石油醚、丙酮、丁酮、氯仿、二氯甲烷、四氯化碳、二硫化碳、DMF、DMSO、苯、甲苯、二甲苯、硝基苯、氯苯、环己烷或正己烷中的1~3种。上述步骤含有双官能团的化合物为含异氰酸酯基的化合物时,所用催化剂为二月桂酸二丁基锡。上述步骤含有双官能团的化合物为含有三嗪基的化合物时,所用催化剂为三乙胺或吡啶。上述步骤含有双官能团的化合物为含有环氧基的化合物时,所用催化剂为氢氧化钠或氢氧化钾。
(3)按反应型阻燃剂与含有双官能团的中间体化合物摩尔比为1:1向三口瓶中加入反应型阻燃剂,补加与步骤(2)等量的催化剂,恒温120℃反应2~12h,得有机高分子定形相变支撑材料。
(4)按比例向三口瓶中加入添加型阻燃剂,混合0.5~2h,蒸发溶剂,真空干燥,即得有机阻燃定形相变储能材料。其中,按质量百分比,有机高分子定形相变支撑材料:80~90wt%,阻燃剂10~20wt%。
表1部分中间体结构与代号
上表中,含有环氧基的中间体化合物中,PEG是指聚乙二醇,后面的数字为其分子量,环氧官能团通过醚键与聚醚相连;含有三嗪基的中间体化合物中PEG是指聚乙二醇,后面的数字为其分子量,三嗪官能团通过醚键与聚醚相连;含有异氰酸酯基的中间体化合物中PEG是指聚乙二醇,后面的数字为其分子量,异氰酸酯官能团通过酯键与聚醚相连。
上述2#~13#化合物按步骤(2)所述方法制备:将聚乙二醇与含有双官能团的化合物按摩尔比1:2溶于甲苯中,并在甲苯中加入对应的催化剂,在N2环境中将上述原料置于带搅拌的三口瓶中,在40℃下反应8h,得含有中间体化合物的甲苯溶液;其中,所述催化剂与聚乙二醇的质量比为1:100;所述甲苯与聚乙二醇的质量比为8.6:1。
下述实施例1~84中记载了进行上述(3)和(4)的步骤。
实施例1
(1)将平均分子量为10000的聚乙二醇及反应型阻燃剂四溴双酚-A在80℃条件下真空干燥48h。
(2)将0.1mol的聚乙二醇(平均分子量10000)与0.2mol的溶于甲苯中,并在甲苯中加入二月桂酸二丁基锡,二月桂酸二丁基锡与聚乙二醇的质量比为1:100;甲苯与聚乙二醇的质量比为8.6:1;在N2环境中将上述原料置于带搅拌的三口瓶中,在40℃下反应8h,得含有双官能团中间体化合物(6#中间体,结构见表1)的甲苯溶液。
(3)按反应型阻燃剂四溴双酚-A与含有双官能团的中间体化合物6#摩尔比为1:1向三口瓶中加入反应型阻燃剂,补加与步骤(2)等量相同的催化剂二月桂酸二丁基锡,恒温120℃反应10h,得有机高分子定形相变支撑材料。
(4)按有机高分子定形相变支撑材料:80wt%,添加型阻燃剂四溴双酚-A:20wt%加入三口瓶中,机械搅拌,混合2h,蒸发溶剂,真空干燥,即得有机阻燃定形相变储能材料。
从材料的红外光谱(附图1)中可以看出,所得有机阻燃定形相变储能材料(聚氨酯/四溴双酚-A)的红外(曲线d)与未添加阻燃剂相变材料(聚氨酯)的红外(曲线c)相比,没有出现新的特征峰,表明两者为物理混合。从材料的XRD表征(附图2)可以看出,所得有机定形相变储能材料的结晶峰与聚乙二醇特征峰相同,具有结晶特性。所得有机定形相变储能材料的DSC曲线(附图3)中,所得聚氨酯/四溴双酚-A有机定形相变储能材料的相变焓值较聚氨酯定形相变支撑材料略低,这是由于物理添加的阻燃剂不具有相变性能。但聚氨酯/四溴双酚-A的相变焓值达到86.71J/g,具有较好相变储热特性。对制得的材料进行极限氧指数测定,聚氨酯有机高分子定形相变支撑材料的极限氧指数为16,而聚氨酯/四溴双酚-A达到19.3,防火性能提高。附图4表明,当温度加热到70℃,聚乙二醇已开始融化,而所得聚氨酯有机高分子定形相变支撑材料和聚氨酯/四溴双酚-A有机阻燃定形相变储能材料即使温度升至95℃,材料仍保持固态,没有流动,表明材料具有优异的定形相变特性。在材料的TG和DTG曲线(附图5)中,可以看到聚氨酯有机高分子定形相变支撑材料和聚氨酯/四溴双酚-A均有两个分解步骤,第一步在250℃左右,为聚氨酯有机高分子定形相变支撑材料中酯键的分解温度,第二步分解在360℃以上,为聚醚的分解温度。因此,实验制得的阻燃定形相变材料热稳定性好,分解温度远高于其相变温度,在应用中有很大的温度范围。聚氨酯/四溴双酚-A的积炭量较聚氨酯有机高分子定形相变支撑材料大,说明添加了四溴双酚-A的有机高分子定形相变支撑材料在燃烧过程中能够产生更多的积炭,在一定程度上达到隔绝燃烧的效果,这也与极限氧指数的结果相符合。
实施例2
利用十溴二苯乙烷代替四溴双酚-A作为添加型阻燃剂,得到相应的有机定形相变储能材料,其他条件与实施例1一致。
实施例3-4
利用2#、3#化合物代替实施例1中的6#中间体,与1#化合物反应,得到相应的有机定形相变储能材料,所用催化剂为氢氧化钠,其他条件与实施例1一致
实施例5-6
利用4#、5#化合物代替实施例1中的6#中间体,与1#化合物反应,得到相应的有机定形相变储能材料,所用催化剂为三乙胺,其他条件与实施例1一致
实施例7-14
利用7-13#化合物代替实施例1中的6#中间体,与1#化合物反应,得到相应的有机定形相变储能材料,其他条件与实施例1一致。
实施例15-26
利用十溴二苯乙烷代替四溴双酚-A作为添加型阻燃剂,得到相应的有机定形相变储能材料,其他条件与实施例3-14一致。
实施例27
将十溴二苯乙烷和四溴双酚-A按质量比1:1混合作为添加型阻燃剂,得到相应的有机定形相变储能材料,其他条件与实施例1一致。
实施例28-33
利用磷酸三(2,3-二氯丙基)酯、聚磷酸铵、磷酸三苯酯、十溴二苯醚、磷酸三(β一氯乙基)酯、磷酸三(β-氯丙基)酯代替四溴双酚-A与定形相变支撑材料掺杂,得到复合型有机阻燃定形相变储能材料,其他条件与实施例1一致。
实施例34
有机高分子定形相变支撑材料:85wt%,添加型阻燃剂四溴双酚-A:15wt%,其他条件与实施例1一致。
实施例35
有机高分子定形相变支撑材料:87wt%,添加型阻燃剂十溴二苯乙烷:13wt%,其他条件与实施例2一致。
实施例36
有机高分子定形相变支撑材料:90wt%,添加型阻燃剂十溴二苯乙烷和四溴双酚-A:10wt%,其他条件与实施例27一致。
实施例37
有机高分子定形相变支撑材料:95wt%,添加型阻燃剂十溴二苯乙烷和四溴双酚-A:5wt%,其他条件与实施例27一致。
实施例38
有机高分子定形相变支撑材料:70wt%,添加型阻燃剂十溴二苯醚和十溴二苯乙烷:30wt%,其他条件与实施例27一致。
Claims (6)
1.一种有机阻燃定形相变储能材料,其特征在于:所述有机阻燃定形相变储能材料由重量百分比为70~95%有机高分子定形相变支撑材料和重量百分比为5-30%的添加型阻燃剂组成;
所述有机高分子定形相变支撑材料的结构通式如下:
m=10~10000的整数;n=10~1000的整数。
2.根据权利要求1所述的一种有机阻燃定形相变储能材料,其特征在于:所述添加型阻燃剂为四溴双酚-A、十溴二苯乙烷、磷酸三(2,3-二氯丙基)酯、聚磷酸铵、磷酸三苯酯、十溴二苯醚、磷酸三(β-氯乙基)酯、磷酸三(β-氯丙基)酯中的1~2种。
3.根据权利要求1所述的一种有机阻燃定形相变储能材料的制备方法,其特征在于:包括以下步骤:
(1)将反应型阻燃剂与如下式所示的聚乙二醇在80℃条件下真空干燥48h;所述反应型阻燃剂为四溴双酚-A;
其中m=10~10000的整数。
(2)将上述聚乙二醇与含有双官能团的化合物按摩尔比1:2溶于溶剂中,并加入催化剂,所述催化剂与聚乙二醇的质量比为1:80~150;N2环境中在40~80℃下搅拌反应2~10h,得含有双官能团的中间体化合物的溶液;所述含有双官能团的化合物为含有环氧结构的化合物;所述溶剂与聚乙二醇的质量比为5~10:1;所述溶剂为四氢呋喃、二氧六环、石油醚、丙酮、丁酮、氯仿、二氯甲烷、四氯化碳、二硫化碳、DMF、DMSO、苯、甲苯、二甲苯、硝基苯、氯苯、环己烷或正己烷中的1~3种;
(3)按反应型阻燃剂与含有双官能团的中间体化合物摩尔比为1:1,将反应型阻燃剂加入到三口瓶中,补加与步骤(2)中等量相同的催化剂,恒温120℃反应2~12h,得有机高分子定形相变支撑材料;
(4)搅拌条件下,将5-30wt%的阻燃剂和70-95wt%的有机高分子定形相变支撑材料混合0.5~2h,蒸发溶剂,真空干燥,即得。
4.一种有机阻燃定形相变储能材料,其特征在于:所述有机阻燃定形相变储能材料由重量百分比为70~95%有机高分子定形相变支撑材料和重量百分比为5-30%的添加型阻燃剂组成;
所述有机高分子定形相变支撑材料的结构通式如下:
V1为Cl、F、NHCH3或NHC4H9;m=10~10000的整数;n=10~1000的整数。
5.根据权利要求4所述的一种有机阻燃定形相变储能材料,其特征在于:所述添加型阻燃剂为四溴双酚-A、十溴二苯乙烷、磷酸三(2,3-二氯丙基)酯、聚磷酸铵、磷酸三苯酯、十溴二苯醚、磷酸三(β-氯乙基)酯、磷酸三(β-氯丙基)酯中的1~2种。
6.根据权利要求4所述的一种有机阻燃定形相变储能材料的制备方法,其特征在于:包括以下步骤:
(1)将反应型阻燃剂与如下式所示的聚乙二醇在80℃条件下真空干燥48h;所述反应型阻燃剂为四溴双酚-A;
其中m=10~10000的整数。
(2)将上述聚乙二醇与含有双官能团的化合物按摩尔比1:2溶于溶剂中,并加入催化剂,所述催化剂与聚乙二醇的质量比为1:80~150;N2环境中在40~80℃下搅拌反应2~10h,得含有双官能团的中间体化合物的溶液;所述含有双官能团的化合物为含有三嗪结构的化合物;所述溶剂与聚乙二醇的质量比为5~10:1;所述溶剂为四氢呋喃、二氧六环、石油醚、丙酮、丁酮、氯仿、二氯甲烷、四氯化碳、二硫化碳、DMF、DMSO、苯、甲苯、二甲苯、硝基苯、氯苯、环己烷或正己烷中的1~3种;
(3)按反应型阻燃剂与含有双官能团的中间体化合物摩尔比为1:1,将反应型阻燃剂加入到三口瓶中,补加与步骤(2)中等量相同的催化剂,恒温120℃反应2~12h,得有机高分子定形相变支撑材料;
(4)搅拌条件下,将5-30wt%的阻燃剂和70-95wt%的有机高分子定形相变支撑材料混合0.5~2h,蒸发溶剂,真空干燥,即得。
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