CN103214499A - Transition metal induced and synthesized Q[8]-alkali metal and alkaline-earth metal ion coordination polymer and synthesis method - Google Patents
Transition metal induced and synthesized Q[8]-alkali metal and alkaline-earth metal ion coordination polymer and synthesis method Download PDFInfo
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Abstract
The invention relates to a transition metal induced and synthesized Q[8]-alkali metal and alkaline-earth metal ion coordination polymer and a synthesis method. In the existence of transition metals, namely, cobalt, copper, nickel and manganese ions, the Q[8]-alkali metal and alkaline-earth metal ion coordination polymer is a Q[8]-alkali metal or alkaline-earth metal lattice coordination polymer which is synthesized by using Q[8] (Cucurbit[8]uril) and an alkali metal ions or alkaline-earth metal ion brine solution under certain conditions. According to the ingredient mole ratio of the Q[8] to the alkali metal salt (or alkaline-earth metal salt) to transition metal ions being 1: (10-16): (2-8), a target compound can be formed by uniformly heating and mixing and standing for a plurality of days at normal temperature. The synthesis method is simple, simple and convenient to operate, short in peroid and the like.
Description
Technical field
Transition metal ion of the present invention induces eight yuan of melon ring-basic metal meshed super molecular polymkeric substance of synthetic and synthetic method thereof to belong to metal-organic supermolecular polymkeric substance and synthetic method field thereof.Be exactly that transition metal ion is induced eight yuan of melon ring-basic metal meshed super molecular polymkeric substance and synthetic methods thereof of synthetic specifically.Eight yuan of melon rings and alkalimetal ion form stratum reticulare structure supermolecule polymer in the present invention.These characteristics might be used for absorption and isolation technique.
Background technology
Metal-organic framework compound (MOF) is the mixture that a class has special frames and nano pore structure in the ligand polymer, be meant inorganic metal center and organo-functional group, connect the crystalline state porous material of constructing jointly mutually with regular pore canal or void structure by coordinate bond or ion-covalent linkage.This is in 20 end of the centurys, a class brand-new material that occurs in Materials science and the inorganic coordination chemistry crossing domain.The MOF material is born from its and just enjoys the expert of numerous areas and scholar's great attention (it relates to chemistry, physics, materialogy etc.) in the world, and develops rapidly and become one of research focus interdisciplinary.This class material not only has the crystalline structure similar to zeolite molecular sieve, and its structure has and can design and cutting, and orientation design and organic selection by topological framework can obtain different size and the duct that need not construct or hole.These special constitutional featuress have a wide range of applications the metal-organic framework compound in research fields such as parting material, the sorbing material with property, sensing material and even energy storage material.
Melon ring (Cucurbit[
n] urils, Q[
n] s) have by n glycosides urea unit and 2n the big ring cage compound that methylene bridge links up, two opening end edge " is inlayed " and a circle carbonylic oxygen atom, thereby has an ability that forms title complex with metallic ion coordination, can be used as organic ligand and metal ion by direct coordination can construct form various metal-organic framework compounds of melon cyclic group with multiple constitutional features (Metal-Organic Framework, MOF).And by inducing action construct melon cyclic group metal-organic framework compound with multidimensional multilayered structure feature (Metal-Organic Framework, MOF) or ligand polymer be the brand-new research direction that Guizhou Province's macrocyclic chemistry and supramolecular chemistry key lab (being called for short key lab later on) newly open up in melon cyclisation field in recent years.
Melon cyclic group metal-organic framework compound (Metal-Organic Framework, MOF) or the present Research of melon cyclic group ligand polymer.The research of melon cyclic group ligand polymer starts from 1999 the earliest, Korea S scholar Kim professor's study group take the lead in having reported the first construct to form with the direct coordination of basic metal rubidium ion by hexa-atomic melon ring (Q[6]) have ... Rb
+-Q[[6]-Rb
+-Q[[6]-Rb
+-Q[[6] ... the ligand polymer of linear structure is further constructed by these linear ligand polymer and to be formed the supramolecule self-assembly entity with nanometer honeycomb structure.After this some odd correlative study reports are arranged closely during the decade once in a while.Key lab reported first in 2008 construct to form by substituted five-membered melon ring of alkyl and the direct coordination of potassium ion have 2 and 3 dimensional organization Q[5]-the metal supermolecular polymkeric substance, opened our laboratory prelude thus in melon cyclic group metal-organic framework compound or the research of melon cyclic group ligand polymer.In recent years, we have found a series of melon cyclic group metal-organic framework compound and their synthetic method.Construct ligand polymer by direct coordination except utilizing alkyl to replace melon ring (alkyl push away the coordination ability that electronic effect has strengthened melon ring and metal ion) with nanostructure, also successively finding and developed organic molecule induces and the synthetic method of inorganic molecule inductive melon cyclic group metal-organic framework compound, since 2010, key lab has applied for a series of by inducing the patent of tactful synthetic melon cyclic group metal-organic supermolecular polymkeric substance and synthetic method thereof continuously, as " class has multi-level porous cave cancellated melon cyclic group metal-organic framework polymkeric substance and synthetic method thereof ", the patent No. 201010204118.8; " the multi-level netted organic framework polymer of class basic metal-melon ring and synthetic method and application ", the patent No. 201010259839.9; " organic molecule is induced five yuan of melon ring-rare earth metal supermolecule polymer and synthetic methods thereof of synthetic ", the patent No. 201010560745.5; " organic molecule is induced synthetic multidimensional porous cave melon cyclic group metal organic frame polymkeric substance and synthetic method ", application number is 201010560740.2; " transition metal ion is induced five yuan of melon ring-rare earth metal meshed super molecular polymkeric substance and synthetic methods thereof of synthetic ", application number is 201010611053.9; " the cadmium cl anion is induced and is constructed seven yuan of melon ring-rare earth metal linear polymer and synthetic methods thereof ", application number is 201110388587.4; " tetrachloro zincic acid negatively charged ion is induced and is constructed seven yuan of melon ring-rare earth metal linear polymer and synthetic methods thereof ", application number is 201210454578.5; " a kind of synthetic hexa-atomic melon ring-rare earth metal linear polymer that utilizes separates the method for weight rare earth ", application number is 201210457330.4 or the like, these patents or patent application have reflected melon cyclic group metal-organic framework compound or melon cyclic group ligand polymer diversity, novelty and singularity, and given the powerful vitality of this emerging research direction, and the more important thing is, the multi-level melon cyclic group of these multidimensional metal-organic framework compound and melon cyclic group ligand polymer have multifarious structure and form, bigger specific surface area and porosity, characteristics such as cutting and nano pore structure are in fractionation by adsorption, gas storage, molecular recognition, photoelectric properties, the magnetic conduction, transmitter, biosimulation, aspects such as microreactor have the prospect of using widely.Present patent application is utilized the inducing action of inorganic molecule, eight yuan of melon rings and basic metal or the direct coordination of earth metals ion is constructed form the stratum reticulare shape supermolecule polymer with special nanostructure.
Summary of the invention
The objective of the invention is to inducing action, the synthetic eight yuan of melon ring-basic metal of design or alkaline-earth metal stratum reticulare shape ligand polymer and synthetic method by transition metal ion.
Transition metal of the present invention is induced synthetic Q[8]-basic metal, alkaline-earth metal ions ligand polymer, be in the presence of transition metal ion, eight yuan of melon ring-basic metal of synthetic or alkaline-earth metal stratum reticulare shape ligand polymer under certain condition in the hydrochloric acid soln of eight yuan of melon rings and basic metal or alkaline-earth metal ions.The chemical formula of eight yuan of melon rings of indication (Q[8]) is
C 48 H 48 N 32 O 16 , structural formula is as follows:
Transition metal of the present invention is induced synthetic Q[8]-basic metal or alkaline-earth metal ions ligand polymer, eight yuan of melon rings of indication and alkalimetal ion or alkaline-earth metal ions form ligand polymer chemical constitution general formula and are:
{[M
x(H
2O)
y·a(C
6H
6N
4O
2)
n]·bCl·cH
2O}
M represents basic metal or alkaline-earth metal ions, and x is quantity 2≤x≤4 of basic metal or alkaline-earth metal ions; Y is basic metal or alkaline-earth metal ions coordinated water molecular amounts 1≤y≤21; Quantity 1.5≤a≤3 of eight yuan of melon rings in a modular construction; N is the polymerization number of degrees of selected melon ring, and eight yuan of melon ring Q[8 are represented in n=8]; C is quantity 2≤b≤8 of cl anion; D is crystal water molecular amounts 68≤c≤130.
Described ligand polymer is in the presence of inductor transition metals cobalt, copper, nickel, mn ion, eight yuan of melon rings (Cucurbit[8] uril, Q[8]) with the hydrochloric acid soln of alkalimetal ion or alkaline-earth metal ions eight yuan of melon ring-basic metal of synthetic or alkaline-earth metal stratum reticulare shape ligand polymer under certain condition.
The alkalimetal ion of above-mentioned indication is Alkali-Metal Na, Rb ionic nitrate or hydrochloride, and the indication alkaline-earth metal ions is alkaline-earth metal Ca, Sr ionic nitrate or hydrochloride.
The transition metal inductor of above-mentioned indication is Co, Cu, Ni, Mn ionic hydrochloride or nitrate.
Transition metal of the present invention is induced synthetic Q[8]-basic metal or alkaline-earth metal ions ligand polymer, the stratum reticulare shape ligand polymer that eight yuan of melon rings that are meant and Alkali-Metal Na, Rb ion or alkaline-earth metal Ca, Sr ion form.
Transition metal of the present invention is induced synthetic Q[8]-synthetic method of basic metal or alkaline-earth metal ions ligand polymer, it is characterized in that synthetic method follows these steps to carry out with condition:
(1) with Q[8], the nitrate of alkalimetal ion or alkaline-earth metal ions or the nitrate or hydrochloride 1: 10 in molar ratio～16: 2～8 batching weighings respectively of hydrochloride and inductor transition metal ion;
(2) with q.s 6.0 mol/L hydrochloric acid solns above-mentioned three kinds of materials are heated to dissolving fully respectively, are cooled to room temperature;
(3) step (2) inductor transition metal ion hydrochloric acid soln is added in the hydrochloric acid soln of alkalimetal ion or alkaline-earth metal ions mixing;
(4) with step (2) Q[8] hydrochloric acid soln adds in the mixing solutions of step (3), stirs;
(5) leave standstill 1～30 day, separate out crystal.
Transition metal of the present invention is induced synthetic Q[8]-synthetic method of basic metal or alkaline-earth metal ions ligand polymer, it is characterized in that indication transition metal inductor is Co, Cu, Ni, Mn ionic hydrochloride or nitrate.The nitrate of alkalimetal ion or hydrochloride are Na or Rb ionic nitrate or hydrochloride, and the nitrate of the alkaline-earth metal ions of indication or hydrochloride are Ca or Sr ionic nitrate or hydrochloride.
Adopt X-ray single crystal diffraction, analysis means such as IR, DSC-TG to carry out structural characterization to institute's synthetic melon cyclic group supramolecule ligand polymer among the present invention.
The employed synthetic method of patent of the present invention has simple to operate, characteristics such as productive rate height, for this class transition metal ion is induced, eight yuan of melon rings and basic metal or the direct coordination of alkaline-earth metal ions are constructed the carrying out of stratum reticulare shape ligand polymer practical application of formation and are laid a good foundation.
Description of drawings:
Fig. 1 inductor Co
2+Under the existence condition, (a) eight yuan of melon ring Q[8] and Rb
+The crystalline structure of the two-dimension netted metal-organic framework that ion coordination forms, (b) in the two-dimensional mesh one by 6 eight yuan of melon rings by 12 Rb
+The subunit structure that the direct coordination of ion is connected to form, (c) per two Rb with nanoporous
+Ion connects the modular construction that three eight yuan of melon rings form, (d) each eight yuan of melon rings and Rb simultaneously
+Ionic coordination situation, (e and f) Q[8]-Rb
+Parallel accumulation graph between two-dimensional mesh.
Annotate: other transition metal, as the Q[8 of Mn, Cu, the plasma-induced formation of Ni]-Rb
+The Q[8 of two-dimension netted metal organic frame compound and Co ion induction]-Rb
+Two-dimension netted metal organic frame compound is the isomorphous, has identical structure, describes so omitted their crystalline structure here.
Fig. 2 inductor Ni
2+Under the existence condition, (a) eight yuan of melon ring Q[8] and Sr
+The crystalline structure of the two-dimension netted metal-organic framework that ion coordination forms, (b) in the two-dimensional mesh one 8 eight yuan of melon rings are arranged by 8 Sr
2+The subunit structure that the direct coordination of ion is connected to form, (c) a kind of eight yuan of melon rings and Sr in the two-dimensional network structure with nanoporous
2+Ionic coordination situation, (d) another kind of eight yuan of melon rings and Sr in the two-dimensional network structure
2+Ionic coordination situation, (e and f) Q[8]-Sr
2+Parallel accumulation graph between the two-dimensional mesh structure.
Fig. 3 Q[8]-RbCl and Q[8]-SrCl
2Ligand polymer crystalline IR collection of illustrative plates is with pure Q[8] the IR collection of illustrative plates compares, and do not have notable difference.
Fig. 4 Q[8]-RbCl and Q[8]-SrCl
2Ligand polymer crystalline DSC-TG collection of illustrative plates, decomposition temperature is than pure Q[8] high respectively about 20 ℃ and 30 ℃.
Specific implementation method:Embodiment 1: transition metal salt Co (NO
3)
2Induce eight yuan of melon rings and basic metal (hydrochloride) meshed super molecular polymkeric substance to synthesize implementation method.With RbCl is the example explanation:
Take by weighing Q[8 respectively] 100 mg (0.07 mmol), RbCl 80.2 mg (0.7 mmol), Co (NO
3)
26H
2O 38.6 mg (0.14 mmol).Q[8] with 60 ℃ of stirring and dissolving of 10 mL, 6 mol/L HCl heating, make the solution clarification, be cooled to room temperature.RbCl makes the solution clarification with the dissolving of 5 mL, 6 mol/L HCl heated and stirred, is cooled to room temperature.Co (NO
3)
26H
2O makes the solution clarification with the dissolving of 5 mL, 6 mol/L HCl heated and stirred, is cooled to room temperature.With Co (NO
3)
26H
2O solution injects RbCl solution, shakes up, then Q[8] in the mixing solutions of solution before pouring into, shake up once more.Leave standstill a couple of days, light blue transparent sheet-like crystal occurs, productive rate is 21%.Its structural formula is: { [Rb
2(H
2O) 1.5 (C
6H
6N
4O
2)
8] 2Cl70H
2O}
Transition metal Co (NO
3)
2Induce in the architecture of eight yuan of melon rings and basic metal RbCl meshed super molecular polymkeric substance and do not induce metallic cation Co
2+, fill Cl between layer and the layer
-And water molecules.Its infrared spectrum and DSC-TG spectrogram are seen Fig. 3-Fig. 4.
Embodiment 2: transition metal salt MnCl
2Induce eight yuan of melon rings and basic metal (hydrochloride) meshed super molecular polymkeric substance to synthesize implementation method.With RbCl is the example explanation:
Take by weighing Q[8 respectively] 100 mg (0.07 mmol), RbCl 80.2 mg (0.7 mmol), MnCl
24H
2O 105.5 mg (0.5 mmol).Q[8] with 60 ℃ of stirring and dissolving of 10 mL, 6 mol/L HCl heating, make the solution clarification, be cooled to room temperature.RbCl makes the solution clarification with the dissolving of 5 mL, 6 mol/L HCl heated and stirred, is cooled to room temperature.MnCl
2With the dissolving of 5 mL, 6 mol/L HCl heated and stirred, make the solution clarification, be cooled to room temperature.With MnCl
24H
2O solution injects RbCl solution, shakes up, then Q[8] in the mixing solutions of solution before pouring into, shake up once more.Leave standstill a couple of days, the water white transparency tabular crystal occurs, productive rate is 25%.Its structural formula is: { [Rb
2(H
2O) 1.5 (C
6H
6N
4O
2)
8] 2Cl68H
2O}
Transient metal Mn Cl
2Induce in the structure of eight yuan of melon rings and basic metal RbCl meshed super molecular polymkeric substance and do not induce metallic cation Mn
2+, fill Cl between layer and the layer
-And water molecules.
Embodiment 3: transition metal NiCl
2Induce eight yuan of melon rings and basic metal (hydrochloride) meshed super molecular polymkeric substance to synthesize implementation method.With RbCl is the example explanation:
Take by weighing Q[8 respectively] 100 mg (0.07 mol), RbCl 80.2 mg (0.7 mmol), Ni (NO
3)
26H
2O 38.5 mg (0.5 mmol).Q[8] with 60 ℃ of stirring and dissolving of 10 mL, 6 mol/L HCl heating, make the solution clarification, be cooled to room temperature.RbCl makes the solution clarification with the dissolving of 5 mL, 6 mol/L HCl heated and stirred, is cooled to room temperature.Ni (NO
3)
26H
2O makes the solution clarification with the dissolving of 5 mL, 6 mol/L HCl heated and stirred, is cooled to room temperature.With Ni (NO
3)
26H
2O solution injects RbCl solution, shakes up, then Q[8] in the mixing solutions of solution before pouring into, shake up once more.Leave standstill a couple of days, the water white transparency tabular crystal occurs, productive rate is 20%.Its structural formula is: { [Rb
2(H
2O) 1.5 (C
6H
6N
4O
2)
8] 2Cl69H
2O}
Transition metal Ni (NO
3)
2Induce in the structure of eight yuan of melon rings and basic metal RbCl meshed super molecular polymkeric substance and do not induce metallic cation Ni
2+, fill Cl between layer and the layer
-And water molecules.
Embodiment 4: transition metal Ni (NO
3)
2Induce eight yuan of melon rings and alkaline-earth metal (hydrochloride) meshed super molecular polymkeric substance to synthesize implementation method.With SrCl
2Be the example explanation:
Take by weighing Q[8 respectively] 100 mg (0.07 mol), SrCl
2212.2 mg (0.8 mmol), Ni (NO
3)
257.7 mg (0.2 mmol).Q[8] with 60 ℃ of stirring and dissolving of 10 mL, 6 mol/L HCl heating, make the solution clarification, be cooled to room temperature.SrCl
2With the dissolving of 5 mL, 6 mol/L HCl heated and stirred, make the solution clarification, be cooled to room temperature.Ni (NO
3)
2With the dissolving of 5 mL, 6 mol/L HCl heated and stirred, make the solution clarification, be cooled to room temperature.With Ni (NO
3)
2Solution injects SrCl
2Solution shakes up, then Q[8] in the mixing solutions of solution before pouring into, shake up once more.Leave standstill a couple of days, the water white transparency tabular crystal occurs, productive rate is 30%.Its structural formula is: { [Sr
4(H
2O)
213 (C
6H
6N
4O
2)
8] 8Cl130H
2O}
Transition metal Ni (NO
3)
2Induce eight yuan of melon rings and alkaline-earth metal SrCl
2Do not induce metallic cation Ni in the structure of meshed super molecular polymkeric substance
2+, fill Cl between layer and the layer
-And water molecules.Its infrared spectrum and DSC-TG spectrogram are seen Fig. 3-Fig. 4.
Claims (7)
1. transition metal is induced synthetic Q[8]-basic metal or alkaline-earth metal ions ligand polymer, it is characterized in that eight yuan of melon rings of indication and alkalimetal ion or alkaline-earth metal ions form ligand polymer chemical constitution general formula and be:
{[M
x(H
2O)
y·a(C
6H
6N
4O
2)
n]·bCl·cH
2O}
M represents basic metal or alkaline-earth metal ions, and x is quantity 2≤x≤4 of basic metal or alkaline-earth metal ions; Y is basic metal or alkaline-earth metal ions coordinated water molecular amounts 1≤y≤21; Quantity 1.5≤a≤3 of eight yuan of melon rings in a modular construction; N is the polymerization number of degrees of selected melon ring, and eight yuan of melon ring Q[8 are represented in n=8]; C is quantity 2≤b≤8 of cl anion; D is crystal water molecular amounts 68≤c≤130;
Described ligand polymer is in the presence of inductor transition metals cobalt, copper, nickel, mn ion, eight yuan of melon rings (Cucurbit[8] uril, Q[8]) with the hydrochloric acid soln of alkalimetal ion or alkaline-earth metal ions eight yuan of melon ring-basic metal of synthetic or alkaline-earth metal stratum reticulare shape ligand polymer under certain condition.
2. transition metal according to claim 1 is induced synthetic Q[8]-basic metal or alkaline-earth metal ions ligand polymer, the alkalimetal ion that it is characterized in that indication is Alkali-Metal Na, Rb ionic nitrate or hydrochloride, and the indication alkaline-earth metal ions is alkaline-earth metal Ca, Sr ionic nitrate or hydrochloride.
3. transition metal according to claim 1 is induced synthetic Q[8]-basic metal or alkaline-earth metal ions ligand polymer, the transition metal inductor that it is characterized in that indication is Co, Cu, Ni, Mn ionic hydrochloride or nitrate.
4. transition metal according to claim 1 is induced synthetic Q[8]-basic metal or alkaline-earth metal ions ligand polymer, it is characterized in that eight yuan of melon rings of indication and Alkali-Metal Na, Rb ion or alkaline-earth metal Ca, Sr ion form stratum reticulare shape ligand polymer.
5. transition metal according to claim 1 is induced synthetic Q[8]-synthetic method of basic metal or alkaline-earth metal ions ligand polymer, it is characterized in that synthetic method follows these steps to carry out:
(1) with Q[8], the nitrate of alkalimetal ion or alkaline-earth metal ions or the nitrate or hydrochloride 1: 10 in molar ratio～16: 2～8 batching weighings respectively of hydrochloride and inductor transition metal ion;
(2) with q.s 6.0 mol/L hydrochloric acid solns above-mentioned three kinds of materials are heated to dissolving fully respectively, are cooled to room temperature;
(3) step (2) inductor transition metal ion hydrochloric acid soln is added in the hydrochloric acid soln of alkalimetal ion or alkaline-earth metal ions mixing;
(4) with step (2) Q[8] hydrochloric acid soln adds in the mixing solutions of step (3), stirs;
(5) leave standstill 1～30 day, separate out crystal.
6. transition metal according to claim 5 is induced synthetic Q[8]-synthetic method of basic metal or alkaline-earth metal ions ligand polymer, the nitrate or the hydrochloride that it is characterized in that the alkalimetal ion of indication are Na or Rb ionic nitrate or hydrochloride, and the nitrate of the alkaline-earth metal ions of indication or hydrochloride are Ca or Sr ionic nitrate or hydrochloride.
7. transition metal according to claim 1 is induced synthetic Q[8]-synthetic method of basic metal or alkaline-earth metal ions ligand polymer, it is characterized in that indication transition metal inductor is Co, Cu, Ni, Mn ionic hydrochloride or nitrate.
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| CN106902553A (en) * | 2017-03-24 | 2017-06-30 | 贵州大学 | A kind of application for being based on ten yuan of melon ring Supramolecular self assembly bodies and application process |
| CN108371957A (en) * | 2018-03-27 | 2018-08-07 | 吕桂兰 | A kind of method that nano-functional material selective epoxidation prepares cosmetic perfumes intermediate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106902553A (en) * | 2017-03-24 | 2017-06-30 | 贵州大学 | A kind of application for being based on ten yuan of melon ring Supramolecular self assembly bodies and application process |
| CN106902553B (en) * | 2017-03-24 | 2019-10-18 | 贵州大学 | A kind of application and application method based on ten yuan of melon ring Supramolecular self assembly bodies |
| CN108371957A (en) * | 2018-03-27 | 2018-08-07 | 吕桂兰 | A kind of method that nano-functional material selective epoxidation prepares cosmetic perfumes intermediate |
| CN108371957B (en) * | 2018-03-27 | 2021-03-16 | 深圳伊赞泉化妆品有限公司 | Method for preparing cosmetic perfume intermediate by selective epoxidation of nano functional material |
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