CN104755419A - 用于有机单片凝胶的隔热组合物及其用途和制备方法 - Google Patents
用于有机单片凝胶的隔热组合物及其用途和制备方法 Download PDFInfo
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Abstract
本发明涉及一种胶化碳基组合物,用于形成一种能够通过热分解形成多孔单片碳的有机聚合单片凝胶,并涉及该组合物的用途,还涉及一种制备该碳基组合物的方法。根据本发明的组合物基于一种至少部分源自于(聚)酚R和(聚)甲醛F的树脂,具有小于或等于40mW.m-1.K-1的热导率,并且所述胶化碳基组合物包含至少一种水溶性阳离子聚电解质P。一种制备这种组合物的方法,包括:a)为了得到一种基于上述树脂的溶液,在所述至少一种阳离子聚电解质P和催化剂的存在下,将所述(聚)酚R和(聚)甲醛F溶解于一种水溶剂W中进行聚合反应,b)将步骤a)中所得的溶液进行胶化,从而得到一种所述树脂的凝胶,然后c)将步骤b)中所得的凝胶进行干燥,从而得到所述有机聚合单片凝胶。
Description
本发明涉及一种胶化碳基组合物,用于形成一种能够通过热分解形成多孔单片碳的有机聚合单片凝胶,并涉及该组合物的用途,还涉及一种制备该碳基组合物的方法。本发明尤其适用于这些有机凝胶的获得,例如气凝胶;并且适用于这些具有很低密度、大比表面积和高孔隙体积的单片碳的获得,并将其作为超级绝热材料使用(即通常具有小于或等于大约40mW.m-1.K-1的热导率)。
气凝胶是多孔材料,在胶化和随后对凝胶的干燥之后而获得,干燥过程中,作为溶剂的液体已经被替换为气体或气体混合物。这些材料以非常低的密度(或高的孔隙体积)作为热绝缘体的应用是非常具有前景的。这是因为,它们的纳米孔隙使得限制包含在孔中的空气的对流效应成为可能。
然而,很低密度的气凝胶的制备方法是复杂的,这是由于其有限的机械性能,至今不允许常规烘箱干燥,特别是由于烘箱干燥过程中溶剂的蒸发而产生了材料中的内应力,破坏了其纳米结构并产生了宏观裂缝。这就是为何使用超临界CO2进行干燥是生产这些低密度气凝胶的惯用手段。本方法给出了关于纳米结构稳定性的不错的结果,但其具有不利于该气凝胶的制造成本的缺点。
二氧化硅气凝胶,其作为超级热绝缘体的应用已经被进行了最广泛的研究(这些气凝胶可具有大约0.015至0.020W.m-1.K-1的热导率),并没有避免这些结果。于是,采用常规烘箱干燥,这些二氧化硅凝胶将遭受大量的致密化和其纳米结构的损失。此外,这些凝胶的开裂会产生粉末,由于二氧化硅纳米粒子粉末的释放,会带来毒性问题。研究工作已经集中于对其表面化学性质进行改性后的二氧化硅气凝胶的弹性回复效应,还集中于使用惰性基团对硅醇基进行替代,使得其在蒸发干燥之后呈现出可逆致密化成为可能。
该原理已经允许以超级绝热纳米气凝胶的形式进行低密度二氧化硅粉末的工业生产,但是并不允许稳定的单片材料的合成,与大比表面积的有机气凝胶对比,其本身作为超级热绝缘体的使用是很有前景的。
以已知的方式,这些有机气凝胶通常由一种间苯二酚-甲醛RF树脂制备,其具有以下优点:成本低廉,能够得到一种能在水中使用的凝胶,能够具有取决于制备条件各种孔隙率值和密度值(例如,根据试剂R、F和催化剂之间的配比)。此外,这些有机气凝胶能以大比表面积的碳的形式被热分解,具有吸收红外辐射和在高温下具有低热导率的优点。另一方面,这些由前体缩聚而成的化学凝胶是不可逆的并且因此不能被重新利用。此外,在高转化率下,这些凝胶成为疏水的而后沉淀析出,其包含机械应力于这些材料中,并且增加了其易碎性。
至于二氧化硅气凝胶,为了获得很低密度的有机单片气凝胶,对这些气凝胶使用一种足够温和的能避免该纳米结构的破裂或收缩并且能避免比表面积的损失的干燥技术是必要的。这种干燥方法通常是通过与乙醇进行溶剂交换,随后通过超临界CO2法干燥来实施的。例如,文件US-A-4997804提到的一种基于间苯二酚-甲醛树脂制备这种有机单片气凝胶的方法的说明,其使用了借助于溶剂交换并且随后借助于超临界流体的这种干燥方法。
如前所述,该干燥技术的一个主要缺点是其实施复杂并且成本高昂。
本发明的目的之一在于提供一种胶化碳基组合物,形成一种有机聚合单片凝胶,其能通过热解形成可能克服上述所有缺点的超级绝热多孔碳单片(即拥有小于或等于40mW.m-1.K-1的热导率)。
令人意外的是,申请人已经发现实现本发明的目的在于:在水相中,向(聚)酚和(聚)甲醛型的树脂前体添加一系列特定的添加剂,包括一种水溶性的阳离子聚电解质,从而使得获得同时具有大比表面积、很低的密度以及高孔隙体积的单片凝胶或者其热解产物成为可能,并且能够免除通过溶剂交换和超临界流体进行的干燥过程。
为了此目的,一种依照本发明的碳基组合物,其基于一种至少部分来源于(聚)酚R和(聚)甲醛F的树脂,其包含至少一种水溶性阳离子聚电解质P。
应当指出的是,本发明中的结合该阳离子聚电解质的这种组合物能通过使用烘箱干燥被方便地获得,其要比采用超临界CO2的干燥方法更容易实施并且在凝胶的生产成本方面损失更少。事实上,申请人已经发现了这种添加剂使得维持由接下来的烘箱干燥而得到的该凝胶的高孔隙率成为可能,并且使得赋予其非常低的密度以及大比表面积和高孔隙体积成为可能。
该术语“凝胶”是指胶体和液体的混合物,其以一种已知的方式自发地形成或者在催化剂的作用下通过胶体溶液的絮凝和混凝而形成。
该术语“水溶性聚合物”是指一种无需加入添加剂(特别是表面活性剂)就能溶解于水中的聚合物,与水分散性聚合物不同,当其与水混合后能够形成一种分散体。
根据本发明的另外一种特点,所述碳基组合物包含一种所述(聚)酚R和(聚)甲醛F进行的聚合反应的产物,该反应在所述至少一种溶解于该溶剂中的阳离子聚电解质P和一种酸或碱催化剂的存在下,于一种水溶剂W中进行。
优选的是,所述聚合反应的产物可包括:
——所述至少一种质量分数非常低的阳离子聚电解质P,其质量分数为0.2%至2%且优选为0.3%至1%,和/或
——所述至少一种阳离子聚电解质P,具有与所述(聚)酚R和(聚)甲醛F有关的P/(R+F)质量比,其为2%至10%且优选为3%至7%,和/或
——所述至少一种阳离子聚电解质P,具有与所述(聚)酚R、(聚)甲醛F和水溶剂W有关的P/(R+F+W)质量比,其为0.3%至2%且优选为0.4%至1.5%。
所述至少一种聚电解质可以是任何一种完全溶于水且具有低离子强度的阳离子聚电解质。
这种有机聚合物优选自以下基团,包括:季铵盐、聚氯化乙烯基吡啶、聚乙亚胺、聚乙烯基吡啶、聚烯丙胺盐酸盐,聚甲基丙烯酸乙酯基三甲基氯化铵、二甲基氯化铵丙烯酰胺共聚物和它们的混合物。
甚至更优选的是,所述至少一种水溶性阳离子聚电解质P是一种盐,其包括来源于选自聚二甲基二烯丙基卤化铵的季铵盐单元,并且其优选聚二甲基二烯丙基氯化铵或聚二甲基二烯丙基溴化铵。
在作为所述树脂的前体聚合物并且可用于本发明的聚合物之中,可提及的是那些来源于至少一种羟基苯型单体和至少一种甲醛单体的缩聚反应的聚合物。此聚合反应可能涉及两种以上不同的单体,该额外的单体可选羟基苯型。该可用的羟基苯优选二酚或三酚,并且最好选择间苯二酚(1,3-二羟基苯)或者间苯二酚与选自邻苯二酚、对苯二酚和间苯三酚中的另一种化合物的混合物。
例如,使用中可以0.3至0.7的R/F摩尔比采用(聚)酚R和(聚)甲醛F。
根据本发明的另外一种特点,所述碳基组合物可优选400m2/g至1200m2/g之间的比表面积,和/或0.1cm3/g至3cm3/g之间的孔隙体积,和/或3nm至30nm之间的平均孔径,和/或0.04至0.4之间的密度。
根据本发明所述的一种有机聚合单片凝胶,例如一种气凝胶,包含一种如上定义的碳基组合物。
优选的是,通过其热分解获得的该凝胶和该碳单片,可以具有10mW.m-1.K-1至40mW.m-1.K-1之间热导率,例如20至35mW.m-1.K-1之间,该凝胶适用于建筑物的隔热保温。
根据本发明,一种制备如上定义的碳基组合物的方法,包含:
a)为了得到一种基于上述树脂的水溶液,在所述至少一种阳离子聚电解质P和催化剂的存在下,将所述(聚)酚R和(聚)甲醛F溶解于一种水溶剂W中进行聚合反应,
b)将步骤a)中所得的溶液进行胶化,从而得到一种所述树脂的凝胶,然后
c)将步骤b)中所得的凝胶进行干燥,从而得到所述有机聚合单片凝胶。
为了获得该多孔单片碳,将步骤c)中所得的干燥凝胶进行热分解。
如上所述和优选的是,步骤a)可通过使用所述至少一种聚电解质P来实施,该聚电解质P在该组合物中的质量分数为0.2%至2%,和/或P/(R+F)的质量比为2%至10%,和/或P/(R+F+W)的质量比为0.3%and 2%。
同样优选的是,其可能以以下方式进行:
——步骤a)在环境温度下,将所述(聚)酚R和所述至少一种阳离子聚电解质P溶解于所述水溶剂中,该溶剂优选包含水,然后,通过向得到的该溶液中加入所述(聚)甲醛F和所述催化剂,其可以是酸或碱,此后,
——步骤b)通过在烘箱中将所述溶液固化。
借助在步骤a)中可用的催化剂,例如其可以是酸性催化剂:例如盐酸、硫酸、硝酸、乙酸、磷酸、三氟乙酸、三氟甲磺酸、高氯酸、草酸、甲苯磺酸、二氯乙酸或甲酸的水溶液;或者其也可以是碱性催化剂:例如碳酸钠、碳酸氢钠、碳酸钾、碳酸铵、碳酸锂、氨水、氢氧化钾和氢氧化钠。
例如,在步骤a)中可以采用的(聚)酚和水的R/W质量比为0.001至0.07。
优选的是,步骤c)在湿润的空气中进行干燥,例如在烘箱中,无需溶剂交换或超临界流体干燥,从而得到所述有机聚合单片凝胶,(根据合成条件且特别是pH)其具有400m2/g至1200m2/g之间的比表面积,和/或0.1cm3/g至3cm3/g之间的孔隙体积,和/或3nm至30nm之间的平均孔径,和/或0.04至0.4之间的密度。
应当指出的是,根据本发明所述的这种水相制备方法使获得取决于合成条件的可控多孔结构成为可能。因此可能得到一种仅有纳米孔的低密度结构(即其孔径小于50nm),或者选择性地在纳米孔和大孔之间得到一种共存体(即其孔径大于50nm)。
本发明的其他特点、优点和细节将会在阅读下述几个实施例的说明书中出现,其以非限制性说明的方式给出。
依照本发明的制备实施例
下面的实施例说明了两种“控制”有机单片凝胶G0和G0′的制备,根据本发明所述的五种有机单片凝胶G1至G5的制备,还有相应的“控制”多孔碳C0与C0′和根据本发明所述的多孔碳C1至C5的制备,其采用以下物质作为起始试剂:
——来源于Acros Organics公司的间苯二酚(R),纯度98%,
——来源于Acros Organics公司的甲醛(F),纯度37%,
——一种催化剂(C)包含盐酸,用于凝胶G1至G4;包含碳酸钠,用于凝胶G5,并且
——聚二甲基二烯丙基氯化铵(P),纯度35%(在水溶液W中),用于凝胶G1至G5。
这些凝胶G0,G0′和G1至G5的制备如下所述:
在第一步中,该间苯二酚R和该聚电解质P(除了凝胶G0和G0′以外)被溶解在一个盛有水的容器中。此后,在其完全溶解之后,再加入甲醛F。在催化剂C的作用下,将该所得聚合物溶液调节至适当的pH值,规定所有这些操作都在环境温度下进行(大约在22℃)。在第二步中,将所得溶液转入到模具里,随后将其置于90℃的烘箱中24小时,从而进行胶凝作用。
此后该凝胶被干燥:
——在一个85℃和90%湿度的湿润的室内干燥17个小时,从而得到凝胶G0′,G2,G4和G5,或
——在用三氟乙酸进行3天溶剂交换后,接着在无水乙醇中进行4天溶剂交换,此后使用超临界CO2,从而获得气凝胶G0,G1和G3。
最后,将所述有机凝胶G0,G0′和G1至G5在氮气环境中于800℃进行热分解,从而得到该多孔单片碳C0,C0′和C1至C5。
在以下表1中:
——R/F:间苯二酚和甲醛之间的摩尔比,
——R/W:间苯二酚和水之间的质量比,
——P表示聚电解质的质量分数,
——P/(R+F):聚电解质和间苯二酚-甲醛前体之间的质量比,
——P/(R+F+W):聚电解质和补充了水的间苯二酚-甲醛前体之间的质量比,还有
——CO2sc表示使用超临界CO2进行干燥,而非根据本发明所述的可用的烘箱干燥。
该凝胶G0,G2和G4(见表2)的热导率和多孔碳C0,C2和C4(见表3)的热导率是在22℃借助neotim热导仪根据热线法测得的,凝胶G4和相应的多孔碳C4在三点式压缩和张力中表现出的机械性能是在与“控制”二氧化硅气凝胶G0″(见表4)的比较中,采用MTS拉伸/压缩测试仪根据标准ASTM C165-07测得的。
对于每种多孔碳C0、C0′和C1至C5,该比表面积,该孔隙体积和该平均孔径都是使用来自Micromeritics公司的Tristar 3020分析仪测得的(表2)。
表1
表2
有机凝胶 | G0 | G0′ | G1 | G2 | G3 | G4 | G5 |
凝胶密度 | 0.40 | 1 | 0.20 | 0.40 | 0.04 | 0.04 | 0.20 |
凝胶热导率(mW/mK) | 24 | - | - | 26 | - | 24 | - |
表3
多孔碳 | C0 | C0′ | C1 | C2 | C3 | C4 | C5 |
碳的比表面积(m2/g) | 983 | 18 | 1014 | 1080 | 769 | 1170 | 670 |
碳的孔隙体积(cm3/g) | 0.58 | 0.012 | 0.87 | 0.95 | 0.32 | 0.47 | 0.26 |
碳的平均孔径(nm) | 3.6 | - | 10 | 10 | 5.4 | 4.1 | 3.9 |
碳的密度 | 0.40 | 0.90 | 0.20 | 0.40 | 0.04 | 0.06 | 0.20 |
碳的热导率(mW/mK) | 30 | - | - | 33 | - | 29 | - |
该“控制”多孔碳C0与C0′和发明中的C1至C5的比较可清楚的表明,阳离子聚电解质P的添加使得对于所得的低密度,即使使用烘箱干燥也能维持纳米级的结构成为可能,(见多孔碳C2,C4和C5的比表面积、孔隙体积和平均孔径值,它们与C0的这些参数的数量级是一样的)然而,若没有该聚电解质那么使用超临界CO2干燥就是必要的了,以便维持该多孔碳C0的纳米结构。
在这些条件下,根据本发明所述的该纳米结构凝胶G1至G5和碳C1至C5的密度总是小于或等于0.4。
如果pH值被调节到1,这些结果也表明获得低得多的密度(小于或等于0.06)的一种单片材料(见本发明中的凝胶G3与G4和碳C3与C4)是可能的。
最后,由本发明中该凝胶G5和相应的碳C5所得的结果表明该合成也能在弱酸性和甚至略带碱性介质(pH>6)的环境中实施。
表4
*引用自M.A.Aegerter等人,“气凝胶手册”在溶胶凝胶衍生材料和技术中的进展,第22章。
表4表明,与已知的二氧化硅气凝胶的机械性能比起来,本发明所述的该凝胶和多孔碳的机械性能具有非常明显的改进。
Claims (13)
1.一种胶化碳基组合物,用于形成一种能够通过热分解形成多孔单片碳的有机聚合单片凝胶,所述组合物基于一种至少部分源自于(聚)酚R和(聚)甲醛F的树脂,并且具有小于或等于40mW.m-1.K-1的热导率,其特征在于,所述胶化碳基组合物包含至少一种水溶性阳离子聚电解质P。
2.根据权利要求1所述的碳基组合物,其特征在于,其包含所述(聚)酚R和(聚)甲醛F在一种水溶剂W中进行聚合反应的产物,该聚合反应在溶解于该溶剂的所述至少一种阳离子聚电解质P和一种催化剂的存在下进行。
3.根据权利要求2所述的碳基组合物,其特征在于,所述聚合反应的产物包含0.2%至2%质量分数的所述至少一种阳离子聚电解质P。
4.根据权利要求2或3所述的碳基组合物,其特征在于,所述聚合反应的产物包含所述至少一种阳离子聚电解质P,其与所述(聚)酚R和(聚)甲醛F的质量比P/(R+F)为2%至10%。
5.根据权利要求2-4中任一项权利要求所述的碳基组合物,其特征在于,所述聚合反应的产物包含所述至少一种阳离子聚电解质P,其与所述(聚)酚R、(聚)甲醛F和水溶剂W的质量比P/(R+F+W)为0.3%至2%。
6.根据权利要求1-5中任一项权利要求所述的碳基组合物,其特征在于,所述至少一种水溶性阳离子聚电解质P是一种有机聚合物,其选自以下基团,包括:季铵盐、聚氯化乙烯基吡啶、聚乙亚胺、聚乙烯基吡啶、聚烯丙胺盐酸盐,聚甲基丙烯酸乙酯基三甲基氯化铵、二甲基氯化铵丙烯酰胺共聚物和它们的混合物。
7.根据权利要求6所述的碳基组合物,其特征在于,所述至少一种水溶性阳离子聚电解质是一种盐,其包括来源于选自聚二甲基二烯丙基卤化铵的季铵盐单元,并且其优选聚二甲基二烯丙基氯化铵或聚二甲基二烯丙基溴化铵。
8.根据前述权利要求中任一项权利要求所述的碳基组合物,其特征在于,其具有:
——400m2/g至1200m2/g之间的比表面积,和/或
——0.1cm3/g至3cm3/g之间的孔隙体积,和/或
——3nm至30nm之间的平均孔径,和/或
——0.04至0.4之间的密度。
9.前述权利要求中任一项权利要求所述的碳基组合物的用途,其用于建筑物的隔热。
10.一种制备如权利要求1至8所述的碳基组合物的方法,其特征在于其包括:
a)为了得到一种基于上述树脂的溶液,在所述至少一种阳离子聚电解质P和催化剂的存在下,将所述(聚)酚R和(聚)甲醛F溶解于一种水溶剂W中进行聚合反应,
b)将步骤a)中所得的溶液进行胶化,从而得到一种所述树脂的凝胶,然后
c)将步骤b)中所得的凝胶进行干燥,从而得到所述有机聚合单片凝胶。
11.根据权利要求10所述的制备方法,其特征在于,步骤a)可通过使用所述至少一种阳离子聚电解质P来实施:
——该聚电解质P在该组合物中的质量分数为0.2%至2%,和/或
——该聚电解质P与所述(聚)酚R和(聚)甲醛F的质量比P/(R+F)为2%至10%,和/或
——该聚电解质P与所述(聚)酚R、(聚)甲醛F和水溶剂W的质量比P/(R+F+W)为0.3%and 2%。
12.根据权利要求10或11所述的制备方法,其特征在于:
——步骤a)在环境温度下实施,将所述(聚)酚R和所述至少一种阳离子聚电解质P溶解于所述水溶剂中,该溶剂优选包含水,然后,通过向得到的该溶液中加入所述(聚)甲醛F和所述酸性或碱性催化剂,此后,
——步骤b)通过在烘箱中将所述溶液固化而实施。
13.根据权利要求10-12中任一项权利要求所述的制备方法,其特征在于,步骤c)在湿润的空气中进行干燥,例如在烘箱中,无需溶剂交换或超临界流体干燥,从而得到所述有机聚合单片凝胶,其具有:
——400m2/g至1200m2/g之间的比表面积,和/或
——0.1cm3/g至3cm3/g之间的孔隙体积,和/或
——3nm至30nm之间的平均孔径,和/或
——0.04至0.4之间的密度。
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CN109680816A (zh) * | 2019-02-13 | 2019-04-26 | 吴葆永 | 一种控温空气层阻断式绝热超低能耗外墙构造 |
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FR2996849B1 (fr) | 2012-10-17 | 2015-10-16 | Hutchinson | Composition pour gel organique ou son pyrolysat, son procede de preparation, electrode constituee du pyrolysat et supercondensateur l'incorporant. |
EP3105057B1 (fr) * | 2014-02-12 | 2018-11-21 | Hutchinson | Panneau isolant sous vide comportant un aérogel organique |
KR20160146662A (ko) * | 2014-03-04 | 2016-12-21 | 허친슨 | 유기 모노리스 겔을 위한 겔화된 조성물, 이의 사용, 및 이를 제조하는 방법 |
WO2015155423A1 (fr) * | 2014-04-11 | 2015-10-15 | Hutchinson | Procede de preparation d'une composition d'aerogel monolithique organique super isolant thermique, cette composition et son utilisation. |
FR3044739B1 (fr) | 2015-12-02 | 2018-05-18 | Hutchinson | Piece isolante mecanique |
KR102375793B1 (ko) | 2020-05-11 | 2022-03-16 | 울산과학기술원 | 다공성 형상 기억 중합체 및 이의 제조 방법 |
DE202021101441U1 (de) | 2021-03-22 | 2021-06-17 | Hutchinson | Modulare Anordnung |
CN113862706A (zh) * | 2021-10-13 | 2021-12-31 | 天津晨祥丰凯新材料科技有限公司 | 碳气凝胶及其前体的制备方法 |
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US20150267400A1 (en) | 2015-09-24 |
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