A kind of method for purifying metal complex single crystal by ionic liquid

A technology of metal complexes and ionic liquids, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of huge energy consumption and investment, inability to achieve deep purification, etc., and achieve high single crystal purity. , The purification process is environmentally friendly and the process is simple.

Active Publication Date: 2022-07-26
黄勇 +4
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commonly used purification methods, such as precipitation method, recrystallization method, etc., often fail to achieve the effect of deep purification. Generally, the purity can only make the impurity content in the product less than 5%, and it is only suitable for occasions where the nature of the product and the impurity are quite different.
Or use conventional methods to purify high-purity, often energy consumption and investment are huge

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for purifying metal complex single crystal by ionic liquid, the operation steps are as follows:

[0027] Step 1), in the ionic liquid of any one of imidazole, pyridine, pyrrolidine, piperidine, morpholine or imide salt mainly containing carboxyl functional group, such as imidazole ion solution containing carboxyl functional group, or containing carboxyl functional group. In the ionic liquid formed by any one of imidazole, pyridine, pyrrolidine, piperidine, morpholine, imide salt, or imidazole, pyridine, pyrrolidine, piperidine, morpholine, imide salt containing carboxyl functional group In the ionic liquid formed by the combination of any several isomers of any compound, such as the ionic solution of two isomers of imidazole containing carboxyl functional groups, add 50g of metal oxide and stir and mix evenly , the metal oxide selected in this embodiment is rubidium oxide.

[0028] Step 2), heating the above-mentioned uniformly mixed ionic liquid to above 56 °...

Embodiment 2

[0035] A method for purifying metal complex single crystal by ionic liquid, the operation steps are as follows:

[0036] Step 1), in the ionic liquid of any one of imidazole, pyridine, pyrrolidine, piperidine, morpholine or imide salt mainly containing carboxyl functional group, such as pyridine ion solution containing carboxyl functional group, or containing carboxyl functional group. In the ionic liquid formed by any one of imidazole, pyridine, pyrrolidine, piperidine, morpholine, imide salt, or imidazole, pyridine, pyrrolidine, piperidine, morpholine, imide salt containing carboxyl functional group In the ionic liquid formed by the combination of any several isomers of any compound, such as the ionic solution of pyridine isomers containing carboxyl functional groups, add 50g of metal hydroxide and stir and mix evenly , the metal hydroxide selected in this embodiment is ferric hydroxide.

[0037] Step 2), heating the above-mentioned uniformly mixed ionic liquid to above 56 ...

Embodiment 3

[0044] A method for purifying metal complex single crystal by ionic liquid, the operation steps are as follows:

[0045] Step 1), in an ionic liquid containing any one of imidazole, pyridine, pyrrolidine, piperidine, morpholine or imide salts mainly containing carboxyl functional groups, such as a pyrrolidine ion solution containing carboxyl functional groups, or containing carboxyl functional groups In the ionic liquid formed by any one of imidazole, pyridine, pyrrolidine, piperidine, morpholine, imide salt, or imidazole, pyridine, pyrrolidine, piperidine, morpholine, imide salt containing carboxyl functional group In the ionic liquid formed by the combination of any of several isomers of any one compound, for example, in the ionic solution of two isomers of pyrrolidine containing a carboxyl functional group, add 50 g of metal oxide and stir Mix well, and the metal oxide selected in this embodiment is cadmium oxide.

[0046] Step 2), heating the above-mentioned uniformly mix...

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Abstract

The invention discloses a method for purifying a single crystal of a metal complex by an ionic liquid. The steps are 1): adding an excess of a metal oxide or a metal hydroxide to the ionic liquid, and stirring and mixing evenly; 2) : Heating the well-mixed ionic liquid to above 56°C until the metal oxide or hydroxide is no longer dissolved, forming a saturated solution of metal complexes; 3): Cooling the saturated solution of metal complexes to below 56°C ; 4): Adjust the pH or temperature of the saturated solution of metal complexes, and then irradiate the cooled saturated solution to stratification with an ultra-ultraviolet beam; 5): Extract the saturated solution after stratification that is rich in metal complexes 6): The ionic liquid rich in metal complexes is nucleated, and then single crystal is cultured to obtain a single crystal of metal complexes. This method has high production efficiency and low energy consumption, and the obtained metal The complex single crystal has high purity, easy operation, low cost, and the whole process is safe and controllable.

Description

technical field [0001] The invention belongs to the technical field of metal complex single crystal purification, in particular to a method for purifying metal complex single crystals by ionic liquid. Background technique [0002] High-purity alkaline-earth metal complexes are often used as co-solvents in the research and production of luminescent materials, so that the activator can easily enter the matrix lattice, and promote the matrix to form crystals of a certain size. Its dosage is sometimes as high as 25%. In addition to being used as cosolvents, alkaline earth metal complexes are also used in large quantities as a host for luminescent materials. In these cases, the presence of impurities such as iron, cobalt, nickel, copper, zinc, and lead in the compound is often detrimental, and all or part of these impurities need to be selectively removed to the ppm level before use. The commonly used purification methods, such as precipitation method, recrystallization method,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B7/14C30B7/06C30B29/10
CPCC30B7/14C30B7/06C30B29/10
Inventor 黄勇卢国东蔡茜黄刚金伟强
Owner 黄勇
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