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Dispersing and adjusting agent capable of adjusting adjusting lithium graininess and application of same

A technology of metal lithium particles and regulators, which is applied in the field of improved metal lithium melting and dispersing regulators, can solve the problems of unstable effect, less white oil, and difficulty in dispersing and regulating the effect. little effect

Active Publication Date: 2013-11-06
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the actual use process, since the white oil needs to be heated above 200°C, the trace moisture remaining in the white oil after the temperature rise is very small, and it is difficult to play the role of dispersion adjustment
The actual use results show that it has a certain effect on promoting the dispersion of lithium metal, but the effect is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Replace the dispersing tank with a volume of 250 L with argon, add 70 L of white oil, and then add a mixture of 0.001% glycerin and 0.001% phenol based on the volume of white oil into the tank. Heat up the jacket of the dispersing kettle, put 10kg of lithium metal into the kettle, and then replace it with argon for 3 times. After the lithium metal is completely melted, start the high-speed stirring at the same speed as in the basic example to melt and disperse the lithium metal (the same below), and pass through the cooling The temperature of the oil is lowered to 170° C., the stirring is stopped and the temperature is continued to be lowered to obtain a mixed dispersion of metal lithium and white oil with a dispersed particle size of 70-100 μm. The mixed dispersion of lithium metal and white oil is put into the reaction kettle, and reacted with n-butane chloride to obtain n-butyllithium. After filtration and sampling analysis, the finished product of butyllithium with a...

Embodiment 2

[0028] Replace the dispersing kettle with a volume of 250L with argon for 3 times, add 70L of white oil, and then add 0.004% glycerin and 0.004% phenol based on the volume of white oil into the kettle. Heat up the jacket of the dispersing kettle, put 10kg of metal lithium into the kettle, and then replace it with argon for 3 times. After the metal lithium is completely melted, start high-speed stirring to melt and disperse the metal lithium. Cool oil to cool down to 170°C, stop stirring and continue to cool down. A mixed dispersion of metal lithium and white oil with a particle size of 30-70 um was obtained, which was finer than that of the improved example 1. The mixed dispersion of lithium metal and white oil is put into the reaction kettle, and reacted with n-butane chloride to obtain n-butyllithium. After filtration and sampling analysis, the finished product of butyllithium with an activity of more than 99% and a colorless appearance is obtained.

Embodiment 3

[0030] Replace the dispersing tank with a volume of 250L with argon for 3 times, add 70L of white oil, and then add 0.005% of N,N-diethylhydroxylamine based on the volume of white oil into the tank. Heat up the jacket of the dispersing kettle, put 10kg of metal lithium into the kettle, and then replace it with argon for 3 times. After the metal lithium is completely melted, start high-speed stirring to melt and disperse the metal lithium. Cool oil to cool down to 170°C, stop stirring and continue to cool down. A mixed dispersion of lithium metal and white oil with a lithium metal dispersion particle size of 20-80 um is obtained. The mixed dispersion of lithium metal and white oil is put into the reactor, and reacted with n-butane chloride to obtain n-butyllithium. After filtration and sampling analysis, the finished product of butyllithium with an activity of more than 99% and a slightly yellow appearance is obtained.

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Abstract

The invention provides a lithium dispersing and adjusting agent. Organic substance containing hydroxyl group, compound containing phosphate and phosphite, or mixture of the previous two according to arbitrary ratio is used as a graininess adjusting agent. Lithium is melted completely at the temperature of 200-250 DEG C; Lithium is dispersed into tiny liquid drops at the rotation speed of 1500-3000 rpm; Lithium is cooled to 150-170 DEG C, and the obtained Lithium grain after cooling and mixing can be used in the synthesis of alkyl-Lithium. The lithium dispersing and adjusting agent overcomes the deficiency in dispersing Lithium grain technology disclosed by the invention CN 1410207A; the special graininess adjusting agent can adjust the graininess and size of the dispersing of the Lithium grain with a good effect, so that the Lithium yield can be increased.

Description

technical field [0001] The invention relates to an improved metal lithium melting and dispersing regulator. Background technique [0002] Metal lithium is used as raw material to prepare alkyllithium compounds. Generally speaking, lithium particles are prepared by melting method, and then reacted with alkylating reagents to obtain alkyllithium compounds. In order to ensure a certain yield, it is necessary to prepare metal lithium first to obtain 5-100um particles. [0003] Metal lithium is melted under the protection of an inert gas, dispersed in an inert oil by high-speed stirring to obtain metal lithium particles, and then the obtained metal lithium particles are used for subsequent reactions, which has a very mature application in industry. For example, in the synthesis of butyllithium, metal lithium is placed in inert oil and heated to 200-250°C to melt, then disperse with high-speed stirring at 3000-15000rpm, and then cool down to below the melting point to stop stirri...

Claims

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Application Information

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IPC IPC(8): B22F9/06
Inventor 陈韶文朱铁辉杨进万金文
Owner CHINA PETROLEUM & CHEM CORP
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