CN102225899A - 一类基于Dawson型多金属氧酸盐的离子液体及其合成方法 - Google Patents
一类基于Dawson型多金属氧酸盐的离子液体及其合成方法 Download PDFInfo
- Publication number
- CN102225899A CN102225899A CN2011100960816A CN201110096081A CN102225899A CN 102225899 A CN102225899 A CN 102225899A CN 2011100960816 A CN2011100960816 A CN 2011100960816A CN 201110096081 A CN201110096081 A CN 201110096081A CN 102225899 A CN102225899 A CN 102225899A
- Authority
- CN
- China
- Prior art keywords
- ionic liquid
- dawson
- dawson type
- octyl
- type polyoxometalate
- Prior art date
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 40
- 238000001308 synthesis method Methods 0.000 title 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N methylene dichloride Chemical compound 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ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000005342 ion exchange Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 125000002347 octyl group Chemical group 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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
本发明属于化学材料制备技术领域，具体涉及一类基于Dawson型多金属氧酸盐的离子液体及其制备方法。该离子液体是由正-四辛基铵阳离子和Dawson型多金属氧酸盐阴离子组成，具体组成分别为：[(n-C8H17)4N]6X2M18O62，其中X为P、As，M为W、Mo，可作为催化剂或者溶剂。其制备方法先合成所需Dawson型多金属氧酸盐；按一定化学计量比称取正-四辛基溴化铵与Dawson型多金属氧酸盐，分别配制成二氯甲烷溶液和水溶液；将正-四辛基溴化铵的二氯甲烷溶液滴加到Dawson型多金属氧酸盐的水溶液中，搅拌发生离子交换反应。根据本发明所提供的这一类离子液体的制备思路，可以制备不同结构和功能的基于多金属氧酸盐的离子液体。
Description
一类基于Dawson型多金属氧酸盐的离子液体及其合成方
法
技术领域
[0001] 本发明属于化学材料制备技术领域，具体涉及一类基于Dawson型多金属氧酸盐的离子液体及其制备方法。
背景技术
[0002] 离子液体是近年来在绿色化学的框架下发展起来的全新的介质与软功能材料，由于其具有低蒸汽压，热稳定性好，液体状态范围宽，良好的离子导电性等优点，在催化、能源、光学等研究领域被广泛关注。传统的离子液体一般是指在室温或室温附近温度下呈液态的由离子构成的物质，包括有机阳离子和无机阴离子两大部分。影响离子型化合物熔点的一个重要因素是构成化合物的阴阳离子之间的库仑作用力。当阴阳离子电荷密度较低且离子体积较大时，离子间的距离增加，有利于产生低熔点盐，即离子液体。多数情况下，新的功能离子液体的设计是将功能基团赋予阳离子部分，而阴离子部分往往被忽略。多金属氧簇阴离子是一类多核配合物，由于其结构确定，种类多样，尺寸可调，被认为是重要的无机建筑块。由于多阴离子表面电荷离域在阴离子表面，与无机酸阴离子比较，多金属氧酸盐阴离子表面电荷密度大大降低，是形成低熔点离子型化合物很好的阴离子选择。将多金属氧簇作为离子液体的阴离子部分，能够产生性质独特的离子液体。
[0003] 而这类离子液体最独特的性质之一就是在一定的温度范围内具有热致液晶行为。 Dawson型多金属氧簇阴离子在形状上是长棒状的，其长度（约12A )明显大于宽度（约8A )，并具有一定的刚性。当与正-四辛基铵阳离子形成离子液体时，由于正-四辛基铵阳离子的烷基链具有一定的柔软性，被吸引在刚性长棒状的Dawson型多金属氧簇阴离子两端， 因而极易形成液晶相。因此，研究基于多阴离子和长链的季铵盐阳离子构筑的低熔点离子型化合物的热致液晶行为是十分有前景的。
发明内容
[0004] 本发明的目的是提出一类新型的基于Dawson型多金属氧酸盐的离子液体及其制备方法。
[0005] 本发明提供的一类基于Dawson型多金属氧酸盐的离子液体，该离子液体是由正-四辛基铵阳离子和Dawson型多金属氧酸盐阴离子组成，具体组成分别为： [(n-C8H17) 4N]6X2M18062，其中 X 为 P、As，M 为 W、Mo。
[0006] 本发明具体包括以下步骤：
[0007]第一步：按文献（Contant，R. Inorg. Synth. 1990,27,104-111)方法合成所需 Dawson型多金属氧酸盐。
[0008] 第二步：按化学计量比6 ： 1称取正-四辛基溴化铵与Dawson型多金属氧酸盐， 分别配制成二氯甲烷溶液和水溶液。
[0009] 第三步：将正-四辛基溴化铵的二氯甲烷溶液滴加到Dawson型多金属氧酸盐的水溶液中，室温下搅拌120〜240分钟，发生离子交换反应，分出有机相并除去溶剂得到。
[0010] 本发明与现有技术相比有以下显著效果：
[0011] 1、本发明所提供的是一类新型离子液体，丰富了离子液体的新品种。
[0012] 2、根据本发明所提供的这一类离子液体的制备思路，可以制备不同结构和功能的基于多金属氧酸盐的离子液体。
[0013] 3、本发明提供的离子液体的制备采用离子交换反应，所用设备少，步骤简单。此外，以水和常规低毒的有机溶剂作为反应溶剂，反应条件温和，成本较低，对环境无污染，适合于工业生产。
[0014] 4、本发明提供的基于Dawson型多金属氧酸盐离子液体由于阴离子部分是具有催化活性的多金属氧酸盐，可以催化某些有机反应。
[0015] 5、本发明提供的基于Dawson型多金属氧酸盐离子液体在加热冷却过程中会出现介晶相。
[0016] 6、本发明提供的基于Dawson型多金属氧酸盐离子液体可能用做太阳能电池或锂离子电池的电解液。
[0017] 基于Dawson型多金属氧酸盐的离子液体和其他离子液体相比，具有许多不同的物理和化学性质，作为一种基于多金属氧酸盐的离子液体，它保持着多金属氧酸盐的特性， 即同时具有酸性和氧化性，独特的反应场，杂多阴离子的软性等。这些性质将赋予它作为催化剂或者溶剂时以特殊功能。利用它的这些特性，如氧化性、非挥发性、热及化学稳地性以及适当的导电性等诸多特性能在氧化还原、催化、电化学、分离科学、含重金属或核衰变物种的废水处理、有机合成、气体分离乃至物质感测等各方面发挥它们的作用。
[0018] 例如，疏水性的基于Dawson型多金属氧酸盐的离子液体可以在不添加硫醇的状态下将金纳米粒及金纳米棒从水溶液中转移到离子液体内，但若要让这些纳米粒在离子液体内仍能稳定维持其型态，必须添加界面活性剂；再有，一些钼或钯催化的有机反应如 Suzuki及Mille Coupling反应可以转移到离子液体内进行，钯纳米粒子可以在长碳链四极铵离子液体内形成并稳定，待钯纳米粒子形成后，将此溶液调整到欲反应的温度，之后加入反应起使物反应一定时间后即可得到产物，产物及未反应的起始物可利用环己烷萃取出来，残留在离子液体内少量的萃取用溶剂可以在真空下除去，因此离子液体及催化剂都可以再循环使用。
[0019] 总之，作为一类新的离子液体，它不仅为离子液体化学拓宽了新的研究领域，也为定向设计和合成具有特定功能的离子液体材料提供有益的信息。
具体实施方式
[0020] 实施例1 : [ (Ii-C8H17) 4N] 6P#18062离子液体的制备
[0021]按文献方法制备 K6P2W18O62 · XH2O0 (Contant, R. Inorg. Synth. 1990，27，104-111) 按化学计量比1 ： 6称取K6PJ18O62 · XH2O和正-四辛基溴化铵，分别配制成水溶液和二氯甲烷溶液，剧烈搅拌下将正-四辛基溴化铵的二氯甲烷溶液逐滴加到K6P2W18O62 · XH2O水溶液中，混合溶液搅拌120〜240分钟，静置分层，用分液漏斗分出下层有机相并除去二氯甲烷，即得到[(n-C8H17) 4N]6P2W18062离子液体。
[0022]实施例 2 ： [ (n-C8H17) 4N] 6As#1804(1 离子液体的制备[0023]按文献方法制备 K6Aii2W18O62 · XH2O0 (Contant, R. Inorg. Synth. 1990，27，104-111) 按化学计量比1 ： 6称取Na6As2W18O62 · χΗ20和正-四辛基溴化铵，分别配制成水溶液和二氯甲烷溶液，剧烈搅拌下将正-四辛基溴化铵的二氯甲烷溶液逐滴加到K6As2W18O62 ·χΗ20水溶液中，混合溶液搅拌120〜240分钟，静置分层，用分液漏斗分出下层有机相并除去二氯甲烷，即得到[(n-C8H17) 4N]6A&W18062离子液体。
[0024]实施例 3 ： [ (n-C8H17) 4Ν] 6Ρ2Μο18062 离子液体的制备
[0025]按文献方法制备 K6P2W18O62 · XH2O0 (Contant, R. Inorg. Synth. 1990，27，104-111) 按化学计量比1 ： 6称取K6PJ18O62 · XH2O和正-四辛基溴化铵，分别配制成水溶液和二氯甲烷溶液，剧烈搅拌下将正-四辛基溴化铵的二氯甲烷溶液逐滴加到K6P2W18O62 · XH2O水溶液中，混合溶液搅拌120〜240分钟，静置分层，用分液漏斗分出下层有机相并除去二氯甲烷，即得到[(n-C8H17) 4Ν]6Ρ2Μο18062 离子液体。
[0026]实施例 4 ： [ (n-C8H17) 4N] 6As2Mo18062 离子液体的制备
[0027]按文献方法制备 K6A&Mo18062。(Contant, R. Inorg. Synth. 1990，27，104-111)按化学计量比1 ： 6称取K6As2Mo18O62和正-四辛基溴化铵，分别配制成水溶液和二氯甲烷溶液，剧烈搅拌下将正-四辛基溴化铵的二氯甲烷溶液逐滴加到K6As2Mo18O62 · XH2O水溶液中，混合溶液搅拌240分钟，静置分层，用分液漏斗分出下层有机相并除去二氯甲烷，即得到[(n-C8H17) 4Ν]6Α&Μο18062 离子液体。
Claims (2)
1. 一类基于Dawson型多金属氧酸盐的离子液体的制备方法，其特征是具体包括以下步骤：第一步：按文献（Contant，R. Inorg. Synth. 1990，27，104-111)方法合成所需 Dawson 型多金属氧酸盐；第二步：按化学计量比6 ： 1称取正-四辛基溴化铵与Dawson型多金属氧酸盐，分别配制成二氯甲烷溶液和水溶液；第三步：将正-四辛基溴化铵的二氯甲烷溶液滴加到Dawson型多金属氧酸盐的水溶液中，室温下搅拌120〜240分钟，发生离子交换反应，分出有机相并除去溶剂得到。
2.按权利要求1的方法制备的一类基于Dawson型多金属氧酸盐的离子液体，其特征是是由正-四辛基铵阳离子和Dawson型多金属氧酸盐阴离子组成，具体组成分别为： [(n-C8H17) 4N]6X2M18062，其中 X 为 P、As，M 为 W、Mo。
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| CN103073499A (zh) * | 2012-11-30 | 2013-05-01 | 辽宁大学 | 一种萃取法制备铼离子液体的方法 |
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| CN103073499A (zh) * | 2012-11-30 | 2013-05-01 | 辽宁大学 | 一种萃取法制备铼离子液体的方法 |
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| CN104529478A (zh) * | 2014-12-13 | 2015-04-22 | 宁波帝杨电子科技有限公司 | 一种陶瓷烧结助剂及其制备方法 |
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| CN110937995A (zh) * | 2019-12-06 | 2020-03-31 | 西安石油大学 | 混合价四羧酸双核钌构筑的Dawson型磷钨杂多酸盐及其合成方法 |
| CN110937995B (zh) * | 2019-12-06 | 2022-01-04 | 西安石油大学 | 混合价四羧酸双核钌构筑的Dawson型磷钨杂多酸盐及其合成方法 |
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