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Application of Benzoazepine Crown Ether Compounds in Separation of Lithium Isotopes

A technology of lithium isotope and heterocrown ether, which is applied in the field of lithium isotope separation, can solve the problems of complex synthesis route and high cost of extraction agent, and achieve the effects of fast isotope exchange rate, simple operation and simple process.

Active Publication Date: 2017-07-18
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1979, Jepson reported that the exchange system of cryptane [2,2,1] chloroform solution and lithium trifluoroacetate aqueous solution had a large separation coefficient (~1.041), but the synthesis route of the extractant was complicated and the cost was high. If To realize the value of industrial application, appropriate improvements must be made

Method used

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  • Application of Benzoazepine Crown Ether Compounds in Separation of Lithium Isotopes
  • Application of Benzoazepine Crown Ether Compounds in Separation of Lithium Isotopes
  • Application of Benzoazepine Crown Ether Compounds in Separation of Lithium Isotopes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Synthesis and Lithium Isotope Separation Properties of Benzomonaazepine-15-Crown-5. The reaction equation is as follows:

[0025]

[0026] Concrete reaction process is as follows:

[0027] Dissolve 5.0g of 2-chloroethoxyethanol, 4.22g of diglycolamine, and 17.0g of sodium carbonate in 100mL of toluene, heat to reflux, and react for 48h. When the temperature drops to room temperature, filter out sodium carbonate, distill off toluene under reduced pressure, add 200mL of water to the residue and extract with dichloromethane, dry the extract phase with anhydrous sodium sulfate, add 16.7mL, 22.9g of 4-methylbenzenesulfonyl chloride and 100mg of 4-dimethylaminopyridine was reacted at room temperature for 24 hours, then an appropriate amount of dilute hydrochloric acid was added, the organic phase was separated, the aqueous phase was extracted with dichloromethane, the organic phase was washed twice with saturated NaCl aqueous solution, and dried over anhydrous sodium sulf...

Embodiment 2

[0030] Synthesis and lithium isotope separation properties of N-methylbenzomonoazepine-15-crown-5. The reaction equation is as follows:

[0031]

[0032] Concrete reaction process is as follows:

[0033] Dissolve 2 g of benzodiazepine-15-crown-5 in 20 mL of formic acid and 20 mL of formaldehyde solution, heat to reflux, and react for 24 hours. When the temperature drops to room temperature, add an appropriate amount of saturated aqueous sodium bicarbonate solution to make the solution alkaline. Then it was extracted with dichloromethane, the extract phase was washed twice with saturated NaCl aqueous solution, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the crude product, which was purified by silica gel column chromatography to obtain 51.7 g of N-methylbenzodiazepine-15-crown-51.7 g, 1 H-NMR (400MHz, CDCl 3 )δ6.94-6.83(m,4H),4.15-4.12(m,4H),3.90-3.87(m,4H),3.77(t,4H),2.74(t,4H),2.35(s,3H) ppm.

[0034] Dissolv...

Embodiment 3

[0036] Synthesis of N-methoxyethylbenzomonoazepine-15-crown-5 and properties of lithium isotope separation. The reaction equation is as follows:

[0037]

[0038] Concrete reaction process is as follows:

[0039] Dissolve 2g of benzodiazepine-15-crown-5 in 100mL of acetonitrile, add 1.04g of 2-bromoethyl methyl ether, 4.9g of anhydrous cesium carbonate, reflux for 24h, and filter out after the temperature drops to room temperature Cesium carbonate, the solvent was evaporated under reduced pressure, and the crude product was purified by silica gel column chromatography to obtain 1.75g ​​N-methoxyethylbenzodiazepine-15-crown-5, 1 H-NMR (400MHz, CDCl 3 )δ6.94-6.83(m,4H),4.14-4.10(m,4H),3.90-3.84(m,4H),3.77(t,4H),3.47(t,2H),3.33(s,3H) , 2.87(t,4H), 2.78(t,2H)ppm.

[0040]Dissolve N-methoxyethylbenzomonaazepine-15-crown-5 in chloroform to prepare 0.15mol / L chloroform solution as the organic phase, and pass liquid-liquid reaction with 2mol / L lithium trifluoroacetate aqueous s...

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Abstract

The invention discloses application of benzo-azacrown ether compounds to separation of lithium isotopes. The benzo-azacrown ether compounds are selected from monoaza15-crown-5, bisaza15-crown-5, triaza15-crown-5 and bisaza18-crown-6. The benzo-azacrown ether compounds serving as extracting agents are dissolved in organic solvents to prepare organic phases, a lithium trifluoroacetate aqueous solution serves as an aqueous phase, and the lithium isotopes are separated at the room temperature by liquid-liquid extraction. The benzo-azacrown ether compounds are easy to dissolve in the organic solvents, efficient separation of the lithium isotopes can be realized by means of liquid-liquid extraction, and considerable separation factors, simplicity and convenience in operation, quickness in isotope exchange and technical simplicity are realized.

Description

technical field [0001] The invention relates to the technical field of lithium isotope separation, in particular to the application of benzazepine crown ether compounds to separate lithium isotopes. Background technique [0002] Lithium (Li) is the lightest metal element, known as "energy metal" and "important element that pushes the world forward". Lithium metal and its compounds have been widely used in the fields of electronics, metallurgy, chemical industry, medicine, nuclear energy, aerospace and energy. It is estimated that the energy contained in 1kg of lithium is equivalent to about 4000t of standard coal, which can generate at least 10MWh of electricity. [0003] Natural lithium contains two isotopes, the abundance of which is 7.48% of 6Li and 92.52% of 7Li. The difference in properties between 6Li and 7Li is called lithium isotope effect. 6Li and 7Li have distinct but extremely important roles in nuclear reactions. 6Li is bombarded by neutrons to generate tritiu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D59/24C07D273/01
CPCB01D59/24C07D273/01
Inventor 文珂刘华胡文敬胡维波杨雅芬吴信浪
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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