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Method for preparing metal complex

A metal complex, metal technology, applied in copper organic compounds, electrolysis process, organic chemistry and other directions, can solve the problems of difficult final separation of products, environmental pollution and other problems, and achieve the effect of convenient separation and purification, broadening research fields and avoiding pollution.

Inactive Publication Date: 2009-08-05
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] On the one hand, the extensive use of organic solvents has caused great pollution to the environment. On the other hand, due to the introduction of supporting electrolytes, by-products are easily formed, which brings difficulties to the final separation of the products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment one, preparation ionic liquid:

[0033](1) Synthesis of 1-butyl-3-methylimidazolium bromide ([Bmim]Br)

[0034] Take N-methylimidazole (6.80mL) and brominated n-butane (10.00mL) with a molar ratio of 1:1.2 into a round bottom flask, put it in a water tank, and irradiate it with microwaves (replace the water in the water tank in time to prevent water becomes hot), stop the radiation after the liquid in the flask turns from mixed to clear, then repeatedly wash with ether several times to remove excess N-methylimidazole, and finally use a vacuum pump to remove Solvent and water gave [Bmim]Br, a colorless ionic liquid. It should be noted that during the reaction process, if the microwave power is too high, the evaporation loss of the halogenated alkanes will increase, and there may be local overheating to decompose the product; while the microwave power is too low, the effect is weak and the reaction cannot be completed; If the medium water temperature is too h...

Embodiment 2

[0039] Embodiment two: complex [Cu 4 (Nmim) 4 (μ 4 -O)(μ-Br) 6 ] of electrochemical synthesis,

[0040] (1) See attached figure 1 and figure 2 As shown, add N-methylimidazole (1ml) into the anode of the compartment electrolytic cell, stir to make it dissolve in 20mL of ionic liquid [Bmim]Br, add 10mmol ammonium bromide to the cathode of the compartment electrolytic cell, stir to dissolve it In 10mL ionic liquid [Bmim]Br.

[0041] Electrode treatment: Before using the anode metal copper, it is washed with concentrated nitric acid, natural water and distilled water in sequence, then rinsed with acetone, dried and weighed; the metal copper sheet suspended by platinum wire is used as the anode (connected to the electrochemical control instrument) Positive electrode), the platinum sheet suspended by the platinum wire is used as the cathode (connected to the negative electrode of the electrochemical control instrument), and the two platinum wires are respectively passed throu...

Embodiment 3

[0045] Embodiment three: complex [Cu(Nmim) 4 Br]Br H 2 Electrochemical synthesis of O,

[0046] (1) if image 3 As shown, add 10mL ionic liquid [Bmim]Br into a 100mL Schlenk flask, add 1ml N-methylimidazole to the above system, stir to dissolve it in the ionic liquid [Bmim]Br;

[0047] The metal copper sheet suspended by the platinum wire is used as the anode (connected to the positive electrode of the electrochemical control instrument), and the platinum sheet is used as the cathode (connected to the negative electrode of the electrochemical control instrument). The current of the reaction process is provided by the electrochemical controller. The total electricity is measured by a silver coulomb meter connected in series in the circuit.

[0048] See attached Figure 4 As shown, the electrolytic cell was evacuated for one minute, then filled with inert gas Ar gas, and this operation was repeated three times to ensure that the reaction system was under inert atmosphere con...

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Abstract

The invention discloses a method of preparing metal compositions, which comprises the following steps: in an electrochemical reaction system, a metal M is used as a sacrificial anode, platinum or graphite is used as an inert cathode, ionic liquid N is used as an electrolyte, and an organic ligand R is added to the electrolyte to electrochemically synthesize the metal compositions in an inert gas atmosphere. Because the invention adopts the ionic liquid as the electrolyte instead of nonaqueous solvent, and no additional support electrolyte is added so that organic solvent can not pollute the environment, and final products are convenient to separate and purify. In addition, the invention uses a direct electrochemical method to prepare compositions of N-methylimidazole and metal copper to widen the research field of the synthesis and the preparation of the metal compositions, and the generation of metal surface compositions provides potential application prospects for the inhibition of metals and catalytic reactions on electrode surfaces.

Description

technical field [0001] The invention relates to a method for preparing metal complexes, in particular to a method for preparing metal complexes using ionic liquid as electrolyte. Background technique [0002] There are various methods for preparing metal complexes. Among them, the electrochemical synthesis method has the advantages of simple steps, mild operating conditions, easy control of the direction of electrode reaction, and low price of metals in the generated complexes. has been widely applied. [0003] Most of the electrolytic synthesis of metal complexes is carried out on metal electrodes. Generally speaking, they can be regarded as reactions to obtain metal complexes through redox. The electrochemical synthesis of metal complexes mostly uses the "sacrificial" anode method (or electrochemical anodic dissolution method), the metal is anodized and dissolved, and the ligand (HL) is reduced on the cathode to release hydrogen gas, and the coordination reaction is carri...

Claims

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Application Information

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IPC IPC(8): C25B3/12C07F1/08C07D233/58C25B3/13
Inventor 袁亚仙姚建林
Owner SUZHOU UNIV
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