CN106832386B - 一种有机气凝胶及其制备方法和应用 - Google Patents
一种有机气凝胶及其制备方法和应用 Download PDFInfo
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- CN106832386B CN106832386B CN201710012528.4A CN201710012528A CN106832386B CN 106832386 B CN106832386 B CN 106832386B CN 201710012528 A CN201710012528 A CN 201710012528A CN 106832386 B CN106832386 B CN 106832386B
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- 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
- 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
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
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- C08G75/045—Polythioethers from mercapto compounds or metallic derivatives thereof from mercapto compounds and unsaturated compounds
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- 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
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- 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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Abstract
本发明公开了一种有机气凝胶及其制备方法和应用，该有机气凝胶主要由含多个巯基的有机单体或低聚物与含多个乙烯基的有机单体或低聚物按巯基与乙烯基摩尔比为1∶0.5～3溶于醇类、酮类、酰胺类、亚砜、呋喃、腈类或苯类有机溶剂制备而成。本发明的有机气凝胶以低内旋转势垒的C‑S键交联形成三维网络结构，赋予气凝胶很好的柔韧性，同时成块性好、具有多孔结构、比表面积高、热导率低、透光性可调，可应用于不同场合。本发明采用高效的硫醇‑烯点击反应，制备过程简单高效、周期短，无需后续的改性步骤；制成的有机气凝胶可以应用在在建筑节能、石油化工或污水处理等领域。
Description
技术领域
本发明涉及化工材料，具体涉及一种柔韧性有机气凝胶及其制备方法和应用。
背景技术
气凝胶是一种具有三维纳米多孔结构的新材料，具有低密度(0.003～0.8g·cm-3)，高孔隙率(80～99.8％)，高比表面积(200～1000m2·g-1)，低热导率(～0.02W·m-1K-1)等性质，在航空航天、化工、节能建筑、军事、通讯、电子、冶金等应用领域有着十分广阔的前景。然而目前报道最多的二氧化硅气凝胶并未得到广泛应用，这主要是因为二氧化硅气凝胶由弱应变性的Si-O-Si键形成二次球形粒子以链珠状的形式相互连接形成三维网络结构，这种结构导致气凝胶在外力作用下容易断裂破碎，结构坍塌，柔韧性差，应用困难。
美国专利US7078359 B2，US8214980 B2和中国专利CN1803602A、CN101318659A、CN101671030A、CN101973752A采用纤维作为增强相来提高气凝胶的柔韧性。虽然复合气凝胶的柔韧性有所提高，但是纤维直径比气凝胶孔径大得多，导致形成的网络结构不均匀，复合材料存在一定的缺陷。另外，增强相纤维材料与气凝胶基体的兼容性也会影响材料的综合性能。美国Meador等人采用聚合物增强增韧SiO2气凝胶，利用聚合物在SiO2粒子表面形成包覆层，通过增加粒子与粒子之间颈部的宽度来提高气凝胶的力学性能，他们首先在SiO2凝胶表面修饰上特殊的官能团如氨基，通过溶剂交换后将修饰的凝胶浸入到某些有机单体的溶剂中，然后引发聚合和超临界干燥获得聚合物增韧的SiO2气凝胶，如聚脲增韧SiO2气凝胶、环氧增韧SiO2气凝胶、聚苯乙烯增韧SiO2气凝胶等。但是上述方法需要凝胶改性、溶剂交换和单体扩散的过程，制备需要数周时间、效率低。因此，为推动气凝胶的应用，需要开发一种工艺简单、效率高的生产方法制备出综合性能优异的，具有柔韧性的气凝胶。
发明内容
发明目的：针对现有技术存在的问题，本发明提供一种有机气凝胶，该有机气凝胶成块性好、具有多孔结构、比表面积高、柔韧性好、热导率低、透光性可调，是低内旋转势垒的C-S键交联形成三维网络结构。
本发明的另一目的是提供一种有机气凝胶的制备方法，该方法工艺简单、效率高、周期短。
最后，本发明还提供了一种有机气凝胶的应用。
技术方案：为了实现上述目的，如本发明所述的一种有机气凝胶，主要由含多个巯基的有机单体或低聚物与含多个乙烯基的有机单体或低聚物按巯基与乙烯基摩尔比为1:0.5～3溶于醇类、酮类、酰胺类、亚砜、呋喃、腈类或苯类有机溶剂制备而成。
其中，所述含多个巯基的有机单体或低聚物选自4,4'-硫代双苯硫酚、甲苯-3,4-二硫酚、1,2-乙二硫醇、1,3-丙二硫醇、2,3-丁二硫醇、1,5-戊二硫醇、1,6-己二硫醇、1,8-辛二硫醇、1,9-壬二硫醇、1，10-癸二硫醇、3,6-二氧-1,8-辛二硫醇、季戊四醇四巯基丙酸酯、三羟甲基丙烷三巯基丙酯、三聚硫氰酸或六元硫醇低聚物中的至少一种。
所述含多个乙烯基的有机单体或低聚物选自异戊二烯、二烯丙基氨基甲酰氯、1,5-己二烯、二烯丙基二硫、1,5-环辛二烯、二聚环戊二烯、二烯丙基胺、2,4-己二烯、1-甲基-1,4-环己二烯、马来酸二烯丙酯、2,4-癸二烯酸乙酯、二烯丙基硫醚、甲基环戊二烯、2,5-二甲基-2,4-己二烯、2,4-庚二烯醛、2,4-癸二烯酸乙酯、亚油酸、聚丁二烯、五甲基环戊二烯、山梨酸、6-甲基-3,5-庚二烯-2-酮、邻苯二甲酸二丙烯酯、山梨酸酯、柠檬醛、双戊烯、二乙烯基四甲基二硅氧烷、聚乙二醇二甲基丙烯酸酯、1,5-戊二醇二丙烯酸酯、二丙烯酸新戊二醇酯、二丙烯酸1,6-己二醇、二丙烯酸乙二醇酯、三烯丙基胺、异氰脲酸三烯丙酯、乙氧基化三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三丙烯酸酯、四甲基四乙烯基环四硅氧烷或八乙烯基聚倍半硅氧烷中的至少一种。
所述有机溶剂为甲醇、乙醇、丙醇、异丙醇、叔丁醇、丙酮、甲酰胺、乙酰胺、二甲基亚砜、四氢呋喃、N-甲基吡咯烷酮、乙腈、丙腈、甲苯或二甲苯中的至少一种。
上述的有机气凝胶孔径分布为2～500nm，BET比表面积为100～1000m2·g-1，透光率为0～99.9％，表观密度为0.01～0.65g·cm-3，优选为0.05～0.30g·cm-3，可以压缩到自身体积的5％～80％，弯曲角度为5～180°，压缩模量为0.01～20MPa，弯曲模量为0.01～5MPa，热导率为0.01～0.80W·m-1·k-1，优选为0.01～0.04W·m-1·k-1。
本发明所述的有机气凝胶的制备方法，包括如下步骤：
(1)将含多个巯基的有机单体或低聚物与含多个乙烯基的有机单体或低聚物按上述的巯基与乙烯基摩尔比溶于有机溶剂中，配置出均一的溶液；
(2)将步骤(1)配置的溶液进行引发聚合得到凝胶，将凝胶在有机溶剂中进行老化处理，该有机溶剂为步骤(1)中所述有机溶剂中的至少一种；
(3)将步骤(2)老化得到的凝胶进行干燥，制备得到有机气凝胶。
其中，步骤(1)所述的溶液溶质的质量浓度为10～300g/L，溶质为含多个巯基的有机单体或低聚物与含多个乙烯基的有机单体或低聚物。
其中，步骤(2)所述的引发聚合得到凝胶为通过30～120℃加热0.5～24h得到；或者通过在溶液中加入引发剂引发聚合得到，引发剂的用量优选为溶质质量的0.5％～5％；或将上述溶液用波长300～350nm的紫外光照射1-6h得到。
作为优选，所述引发剂为偶氮二异丁腈、偶氮二异庚腈、异丙苯过氧化氢、叔丁基过氧化氢、过氧化二异丙苯、过氧化二叔丁基、过氧化二苯甲酰、过氧化十二酰、过氧化苯甲酸叔丁酯、过氧化二碳酸二异丙酯、过氧化二苯甲酰/N或N-二甲基苯胺中的至少一种。
所述老化处理的温度为30～100℃，时间2～24小时。
所述干燥为超临界CO2干燥、真空冷冻干燥或常压干燥等干燥方法。
本发明所述的有机气凝胶的在建筑节能、石油化工或污水处理领域中的应用。
有益效果：与现有技术相比，本发明具有以下优点：
1、本发明的有机气凝胶以低内旋转势垒的C-S键交联形成三维网络结构，赋予气凝胶很好的柔韧性。
2、本发明的成块性好、具有多孔结构、比表面积高、柔韧性好、热导率低、透光性可调，可应用于不同场合。
3、本发明的有机气凝胶采用高效的硫醇-烯点击反应，制备过程简单高效、周期短，无需后续的改性步骤。
附图说明
图1是实施例1制备的有机气凝胶外观示意图；
图2是实施例3制备的另一种有机气凝胶外观示意图，从图中可以看出气凝胶具有很好的柔韧性；
图3是实施例3制备的有机气凝胶的扫描电镜照片，从图中可以看出气凝胶具有纳米多孔结构。
实施例1
将巯基与乙烯基摩尔比为1:0.5的3,6-二氧-1,8-辛二硫醇和异氰脲酸三烯丙酯混合于乙酰胺溶剂中，溶质的质量浓度为200g/L；将溶液中加入3％的引发剂偶氮二异丁腈搅拌均匀后，静置得到凝胶；将凝胶在30℃下用丙酮浸泡老化24h；然后在80℃的常压环境下干燥24h，得到柔韧性有机气凝胶。
实施例1制备的柔韧性气凝胶的密度为0.25g·cm-3，孔径分布为2～50nm，BET比表面积为800m2·g-1，热导率为0.04W·m-1·k-1，透光率为89.5％，可压缩到自身体积的65％，弯曲角度达150°，压缩模量为1.5MPa，弯曲模量为0.5MPa；其外观示意图如图1所示，从图中能够清楚看到纸张上的字母，从而可以得出气凝胶具有很好的透光性。
实施例2
将巯基与乙烯基摩尔比为1:1的甲苯-3,4-二硫酚和三羟甲基丙烷三丙烯酸酯混合于甲酰胺溶剂中，溶质的质量浓度为50g/L；在溶液中加入0.5％的引发剂异丙苯过氧化氢搅拌均匀后，静置得到凝胶；将凝胶在50℃下用丙酮浸泡老化12h；然后真空冷冻干燥24h，得到柔韧性有机气凝胶。
实施例2制备的柔韧性气凝胶的密度为0.08g·cm-3，孔径分布为2～250nm，BET比表面积为400m2·g-1，热导率为0.02W·m-1·k-1，透光率为0％，可压缩到自身体积的70％，弯曲角度达180°，压缩模量为0.7MPa，弯曲模量为0.1MPa。
实施例3
将巯基与乙烯基摩尔比为1:1的季戊四醇四巯基丙酸酯和异氰脲酸三烯丙酯混合于甲醇溶剂中，溶质的质量浓度为10g/L；将溶液加热到70℃反应10h引发聚合得到凝胶；将凝胶在50℃下用异丙醇浸泡老化24h；然后超临界CO2干燥24h，得到柔韧性有机气凝胶。
实施例3制备的柔韧性气凝胶的密度为0.05g·cm-3，孔径分布为2～50nm，BET比表面积为1000m2·g-1，热导率为0.01W·m-1·k-1，透光率为99.9％，可压缩到自身体积的80％，弯曲角度达180°，压缩模量为0.01MPa，弯曲模量为0.01MPa；其外观示意图如图2所示，从图中可以看出气凝胶可以打结，说明气凝胶具有很好的柔韧性；实施例3制备的有机气凝胶的扫描电镜照片如图3所示，从图3中可以看出气凝胶具有纳米多孔结构。
实施例4
将巯基与乙烯基摩尔比为1:2的季戊四醇四巯基丙酸酯和异氰脲酸三烯丙酯混合于四氢呋喃溶剂中，溶质的质量浓度为100g/L；将溶液在波长300nm的紫外光照射6h引发聚合得到凝胶；将凝胶在50℃下用乙醇浸泡老化20h；然后真空冷冻干燥48h，得到柔韧性有机气凝胶。
实施例4制备的柔韧性气凝胶的密度为0.15g·cm-3，，孔径分布为2～350nm，BET比表面积为220m2·g-1，热导率为0.025W·m-1·k-1，透光率为75.5％，可压缩到自身体积的65％，弯曲角度达140°，压缩模量为1.0MPa，弯曲模量为0.15MPa。
实施例5
将巯基与乙烯基摩尔比为1:3的三羟甲基丙烷三巯基丙酯和邻苯二甲酸二丙烯酯混合于甲醇溶剂中，溶质的质量浓度为300g/L；将溶液在波长350nm的紫外光照射1h引发聚合得到凝胶；将凝胶在70℃下用乙醇浸泡老化8h；然后100℃的常压环境下干燥24h，得到柔韧性有机气凝胶。
实施例5制备的柔韧性气凝胶的密度为0.30g·cm-3，孔径分布为10～500nm，BET比表面积为100m2·g-1，热导率为0.05W·m-1·k-1，透光率为45.3％，可压缩到自身体积的50％，弯曲角度达155°，压缩模量为1.7MPa，弯曲模量为0.6MPa。
实施例6
将巯基与乙烯基摩尔比为1:2.5的三羟甲基丙烷三巯基丙酯和四甲基四乙烯基环四硅氧烷混合于N-甲基吡咯烷酮溶剂中，溶质的质量浓度为150g/L；溶液中加入5％的引发剂过氧化二苯甲酰/N,N-二甲基苯胺搅拌均匀后，静置得到凝胶；将上述凝胶在100℃下用N-甲基吡咯烷酮浸泡老化2h；然后100℃的常压环境下干燥24h，得到柔韧性有机气凝胶。
实施例6制备的柔韧性气凝胶的密度为0.20g·cm-3，孔径分布为10～200nm，BET比表面积为620m2·g-1，热导率为0.025W·m-1·k-1，透光率为85.5％，可压缩到自身体积的75％，弯曲角度达175°，压缩模量为1.1MPa，弯曲模量为0.3MPa。
实施例7
实施例7与实施例3的原料和制备方法相同，不同之处在于溶液加热到30℃反应24h引发聚合得到凝胶。
实施例8
实施例7与实施例3的原料和制备方法相同，不同之处在于溶液加热到120℃反应0.5h引发聚合得到凝胶。
实施例9
将实施例1至7制备的聚合物笼状倍半硅氧烷杂化气凝胶在建筑节能、高温隔热、石油化工或污水处理等领域中应用。
试验例1
通过对本发明实施例1至3制备的有机气凝胶的各项指标进行检测，包括密度、热导率、柔韧性(实施例1至3制备的有机气凝胶可压缩到自身体积65～80％，弯曲角度达150～180°，压缩模量0.01～1.5MPa，弯曲模量0.01～0.5MPa)数据见各个实施例。同时将各个实施例与对比例进行对比，结果见表1。
对比例1采用实施例1的原料和方法，不同之处在于巯基与乙烯基摩尔比为1:0.4。
对比例2采用实施例1的原料和方法，不同之处在于巯基与乙烯基摩尔比为1:3.1。
表1有机气凝胶的各项指标
由表1可知，实施例1至3制备的有机气凝胶与对比例相比，本发明制备的有机气凝胶其密度更低、热导率更低，并且柔韧性大大提高。
Claims (10)
1.一种柔韧性有机气凝胶，其特征在于，主要由含多个巯基的有机单体或低聚物与含多个乙烯基的有机单体或低聚物按巯基与乙烯基摩尔比为1：0.5~3溶于醇类、酮类、酰胺类、亚砜、呋喃、腈类或苯类有机溶剂制备而成；所述有机气凝胶以低内旋转势垒的C-S键交联形成三维网络纳米多孔结构；
所述的有机气凝胶的制备方法，包括如下步骤：
（1）将含多个巯基的有机单体或低聚物与含多个乙烯基的有机单体或低聚物按上述的巯基与乙烯基摩尔比溶于有机溶剂中，配置出均一的溶液；
（2）将步骤（1）配置的溶液进行引发聚合得到凝胶，将凝胶在有机溶剂中，进行老化处理，该有机溶剂为步骤（1）中所述有机溶剂中的至少一种；
（3）将步骤（2）老化得到的凝胶进行干燥，制备得到有机气凝胶。
2.根据权利要求1所述的柔韧性有机气凝胶，其特征在于，所述含多个巯基的有机单体或低聚物选自4, 4'-硫代双苯硫酚、甲苯-3, 4-二硫酚、1, 2-乙二硫醇、1, 3-丙二硫醇、2, 3-丁二硫醇、1, 5-戊二硫醇、1, 6-己二硫醇、1, 8-辛二硫醇、1, 9-壬二硫醇、1，10-癸二硫醇、3, 6-二氧-1, 8-辛二硫醇、季戊四醇四巯基丙酸酯、三羟甲基丙烷三巯基丙酯、三聚硫氰酸或六元硫醇低聚物中的至少一种。
3.根据权利要求1所述的柔韧性有机气凝胶，其特征在于，所述含多个乙烯基的有机单体或低聚物选自异戊二烯、二烯丙基氨基甲酰氯、1, 5-己二烯、二烯丙基二硫、1, 5-环辛二烯、二聚环戊二烯、二烯丙基胺、2, 4-己二烯、1-甲基-1, 4-环己二烯、马来酸二烯丙酯、2, 4-癸二烯酸乙酯、二烯丙基硫醚、甲基环戊二烯、2, 5-二甲基-2, 4-己二烯、2, 4-庚二烯醛、2, 4-癸二烯酸乙酯、亚油酸、聚丁二烯、五甲基环戊二烯、山梨酸、6-甲基-3, 5-庚二烯-2-酮、邻苯二甲酸二丙烯酯、山梨酸酯、柠檬醛、双戊烯、二乙烯基四甲基二硅氧烷、聚乙二醇二甲基丙烯酸酯、1, 5-戊二醇二丙烯酸酯、二丙烯酸新戊二醇酯、二丙烯酸1,6-己二醇、二丙烯酸乙二醇酯、三烯丙基胺、异氰脲酸三烯丙酯、乙氧基化三羟甲基丙烷三丙烯酸酯、三羟甲基丙烷三丙烯酸酯、四甲基四乙烯基环四硅氧烷或八乙烯基聚倍半硅氧烷中的至少一种。
4.根据权利要求1所述的柔韧性有机气凝胶，其特征在于，所述有机溶剂为甲醇、乙醇、丙醇、异丙醇、叔丁醇、丙酮、甲酰胺、乙酰胺、二甲基亚砜、四氢呋喃、N-甲基吡咯烷酮、乙腈、丙腈、甲苯或二甲苯中的至少一种。
5.一种如权利要求1所述的柔韧性有机气凝胶的制备方法，其特征在于，包括如下步骤：
（1）将含多个巯基的有机单体或低聚物与含多个乙烯基的有机单体或低聚物按上述的巯基与乙烯基摩尔比溶于有机溶剂中，配置出均一的溶液；
（2）将步骤（1）配置的溶液进行引发聚合得到凝胶，将凝胶在有机溶剂中，进行老化处理，该有机溶剂为步骤（1）中所述有机溶剂中的至少一种；
（3）将步骤（2）老化得到的凝胶进行干燥，制备得到有机气凝胶。
6.根据权利要求5所述的制备方法，其特征在于，步骤（1）所述的溶液溶质的质量浓度为10~300g/L，溶质为含多个巯基的有机单体或低聚物与含多个乙烯基的有机单体或低聚物。
7.根据权利要求5所述的制备方法，其特征在于，步骤（2）所述的引发聚合得到凝胶为通过30~120℃加热0.5~24h得到；或者通过在溶液中加入引发剂引发聚合得到，引发剂的用量为溶质质量的0.5%~5%；或将上述溶液用波长300~350nm的紫外光照射1-6 h得到。
8.根据权利要求5所述的制备方法，其特征在于，步骤（2）所述老化处理的温度为30~100℃，时间2~24小时。
9.根据权利要求5所述的制备方法，其特征在于，步骤（3）所述干燥为超临界CO2干燥、真空冷冻干燥或常压干燥。
10.一种如权利要求1所述的柔韧性有机气凝胶的在建筑节能、石油化工或污水处理领域中的应用。
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