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化学进展 2020, Vol. 32 Issue (8): 1158-1171 DOI: 10.7536/PC200433 前一篇   后一篇

• 综述 •

无溶剂或少溶剂的固态化学反应

雷立旭1,*(), 周益明2   

  1. 1.东南大学化学化工学院 南京 211189
    2.南京师范大学化学与材料科学学院 南京 210023
  • 收稿日期:2020-02-28 修回日期:2020-03-22 出版日期:2020-08-24 发布日期:2020-04-23
  • 通讯作者: 雷立旭
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Solvent-Free or Less-Solvent Solid State Reactions

Lixu Lei1,*(), Yiming Zhou2   

  1. 1. School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189, China
    2. School of Chemistry and Materials Science, Nanjing Normal University, Nanjing 210023, China
  • Received:2020-02-28 Revised:2020-03-22 Online:2020-08-24 Published:2020-04-23
  • Contact: Lixu Lei
  • About author:
    * e-mail:

根据热力学,固态化学反应一般具有一旦发生就必完全的特征;但在固体之间存在组成可连续变化的溶液(固熔体)时,固态化学反应体系有可能出现化学平衡。固态化学反应还可能导致立体选择性产物、产物颗粒不易长大、最低反应温度等特征。本文特别指出,为了促进固态化学反应快速、有效、安全地发生,可使用少量溶剂而不用担心固态化学反应无平衡特征的丧失,同时获得良好流动性的反应物浆料,并因此能使用适当的搅拌技术来促进反应;其次,任何复杂的固态化学反应都可以分解成若干双组分反应,可以按一定步骤实现复杂化合物的合成或装配。因此,研究固态化学反应可能会产生更加绿色的化学过程,具有非常现实的理论和应用价值。本文以固态配位化学反应为例来说明如上理论推演结果。这里,固态配位化学反应是固体无机金属化合物与固体有机或无机配体之间的化学反应,它们与固态有机化学反应一样,可以在室温~300 ℃的温度下、不存在任何溶剂的情况下发生。

关键词： 凝聚态化学, 固态配位化学反应, 少溶剂反应, 绿色化学

According to thermodynamics, solid state reactions will generally proceed to their 100% completion once they start; however, they may stop at the equilibrium state in case that there is a solid solution with continuously changing concentration. Solid state reactions also have the following characteristics:(1) they could produce stereoselective products;(2) the particle size of the products could be very small(nano-sized);(3) there is the lowest temperature for the reaction to be initiated. Here, it is particularly pointed out that a little solvent can be employed to accelerate solid state reactions with consequent safety and effectivity, but not the equilibrium; also, the solvent can make the solid mixture more fluidized, thus the mass transportation can be speeded up by a proper blender. In addition, solid state reactions can be used to assemble materials step by step, since any complex reactions can be decomposed to a series of reactions of two reactants. Consequently, studies on solid state reactions can lead to greener chemical processes. All those are demonstrated in this paper with solid state coordination reactions, which are the reactions of solid inorganic metal compounds and solid organic or inorganic ligands. The solid state coordination reactions are well known that they take place at near room temperature up to 300 ℃ without the help of solvents, just like the solid state organic reactions.

Contents

1 Introduction: how to develop a greener chemical process

1.1 Definition of greener chemical process

1.2 Greener chemical processes based on solid-state reactions

1.3 Brief history of solid-state coordination reactions

2 Physical chemistry of solid-state reactions

2.1 Thermodynamics of solid-state reactions

2.2 Thermodynamics of less solvent reactions

2.3 Kinetics of solid-state reactions

3 Syntheses based on solid-state coordination reactions

3.1 Syntheses based on non-solvation

3.2 Syntheses of nanoparticles based on diffusion difficulty in solids

4 Less solvent reactions and their applications in industrialization of solid-state reactions at near room temperatures

4.1 Examples of a few less solvent reactions

4.2 Problems in industrialization of solid-state reactions at near room temperatures

5 Conclusion and outlook

Key words: condensed state chemistry, solid state coordination reaction, less solvent reaction, green chemistry
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图1 化学反应的Gibbs自由能与溶剂用量关系的示意图。处于底部的蓝色曲线是溶液反应的,必定存在平衡;绿色勺型曲线是少溶剂反应,在反应即将结束时可能会出现平衡。此时减少溶剂的量会使体系的自由能沿着虚线前进;红色直线是无溶剂的固态化学反应的情况,其中没有化学平衡
Fig.1 The relationship of Gibbs free energy of the system to the amount of solvent used. The blue curve at the bottom is for the solution reaction, in which there is an equilibrium point; the red straight line at the top is for solvent-free solid state reaction, where there will be no equilibrium; and the green spoon-like curve in the middle correspond to the less solvent reaction, which may follow the dashed line if the solvent is removed at the end of the reaction
图2 银的体扩散系数Db、晶界扩散系数Dg和表面扩散系数Ds与温度的关系[16]
Fig.2 The diffusion coefficients of silver for bulky dif-fusion Db, grain boundary diffusion Dg and surficial dif-fusion Ds[16]
图3 CuCl2·2H2O与2,2'-联吡啶的反应(重新组合的文献[43]原图)。A:(a)反应开始反应物团聚时的XRD,此时存在Cu(bipy)Cl2的衍射峰(数字标出的峰)、bipy和最终产物的峰;(b)反应结束后的XRD。B和C:反应物按1∶1和1∶2摩尔比混合时反应的DSC曲线。D:曲线b是Cu(bipy)Cl2与bipy按1∶1摩尔比混合时反应的DSC曲线
Fig.3 Data from the reaction of CuCl2·2H2O and 2,2'-bipyridyl (adapted from ref[43]). A: XRD pattern of (a) the reaction mixture of 1∶2 molar ratio when it aggregated, in which diffraction peaks of Cu(bipy)Cl2 can be found; (b) the final product; B: DSC curve of the 1∶1 reaction; C: DSC curve of the 1∶2 reaction; and D: DSC curves of the 1∶1 reaction (a) and Cu(bipy)Cl2 and bipy in 1:1 molar ratio
图4 FeSO4·7H2O与邻菲咯啉按1∶1摩尔比的固态化学反应[45]。A:几种物质的XRD谱(a)邻菲咯啉;(b)FeSO4·7H2O;(c)Fe(H2O)3(phen)SO4;(d)Fe(H2O)3(phen)SO4·5H2O;B:Fe(H2O)3(phen)SO4·5H2O和邻菲咯啉按1∶2摩尔比反应时的初始混合物(a)和反应产物(b)的XRD谱;C:FeSO4·7H2O与邻菲咯啉按1∶1摩尔比反应时的EDXRD随时间的变化;D:不同温度下中间产物和最终产物的XRD主峰强度变化
Fig.4 Data of the solid state reaction of FeSO4·7H2O and o-phenanthroline[45]. A: XRD patterns of (a) phen;(b)FeSO4·7H2O;(c)Fe(H2O)3(phen)SO4;(d)Fe(H2O)3(phen)SO4·5H2O;B:XRD patterns of the initial reaction mixture of Fe(H2O)3(phen)SO4·5H2O and phen in 1∶2 molar ratio (a) and the final (b);C:The EDXRD of the solid state reaction of FeSO4·7H2O and phen in 1∶1 molar ratio as a function of time;D:The intensity of main XRD peak as the function of time at different temperatures
图5 固态化学反应中反应物和产物的颗粒随时间变化的示意图
Fig.5 The changes of particles of reactants and products during a solid state reaction
图6 固体(NH4)2MoS4与固体CuX(X = Cl、Br、I、CN、SCN)反应得到的2核到7核原子簇骨架结构示意图[49, 52]
Fig.6 The framework of 2 ~ 7 nuclear clusters formed from the reaction of (NH4)2MoS4 and CuX(X = Cl, Br, I, CN, SCN)[49, 52]
图7 [Mg(H2O)6]Cl2和NH4[Mg(H2O)6]Cl3晶体中的Mg(H2O)62+(八面体结构)、Cl-(绿球)和NH4+(蓝球)。为简单故,图中略去了氢原子。(a)[Mg(H2O)6]Cl2;(b)NH4[Mg(H2O)6]Cl3
Fig.7 The octahedral Mg(H2O)62+, Cl-(green ball) and NH4+ (blue ball) in crystals of (a)[Mg(H2O)6]Cl2 and (b) NH4[Mg(H2O)6]Cl3
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摘要

无溶剂或少溶剂的固态化学反应