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Methyllithium solution and preparation method thereof

A technology of methyl lithium and solution, which is applied in the field of preparation of methyl lithium solution, can solve the problems of comprehensive cost affecting product market competitiveness, high price of methyl tetrahydrofuran, and difficulty in solvent recovery and separation, so as to reduce production cost and improve safety High efficiency and high reaction yield

Inactive Publication Date: 2015-12-16
JIANGSU CHANGJILI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The U.S. patent discloses the production of methyllithium in tetrahydrofuran and aromatic hydrocarbon solvents containing methyltetrahydrofuran. The stability of methyllithium produced by tetrahydrofuran as a solvent is relatively poor, and the production of methyllithium from aromatic hydrocarbon solvents containing methyltetrahydrofuran can increase the stability of methyllithium. Stability, but the toxicity of aromatic solvents is high, the price of methyl tetrahydrofuran is high, the recovery and separation of solvents is difficult, and the comprehensive cost affects the market competitiveness of products

Method used

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  • Methyllithium solution and preparation method thereof
  • Methyllithium solution and preparation method thereof
  • Methyllithium solution and preparation method thereof

Examples

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Effect test

Embodiment 1

[0035] Under normal pressure at 20-40°C and under the protection of inert gas argon, 21g of metal lithium sand is wrapped with 50g of diethoxymethane and poured into a closed reactor, and the remaining 900g of diethoxymethane is mixed with 105g of lithium bromide and then added In the reactor, add 75g of methyl chloride into the reactor within 1 hour, and the reactor is cooled with a low-temperature refrigerant interlayer, and the temperature is controlled at 20-40°C. After the mixture is added, it is kept at 30-40°C for 1 hour, and the quality of methyllithium is obtained by filtration. A methyllithium solution with a fraction of 3.03% and a mass fraction of lithium bromide of 9.65% was named sample No. 1, and the yield of methyllithium was 98.9%.

Embodiment 2

[0037] Under normal pressure at 20-40°C and under the protection of inert gas argon, 63g of metal lithium sand was wrapped with 63g of diethoxymethane and poured into a closed reactor, 300g of lithium bromide was quickly added to metal lithium, and then the remaining 437g Diethoxymethane was added to the reactor, and 225g of methyl chloride was added to the reactor within 4 hours. The reactor was cooled with a low-temperature refrigerant interlayer, and the temperature was controlled at 20-40°C. After the mixture was added, it was kept at 30-40°C for 2 hours, and filtered A methyllithium solution with a mass fraction of methyllithium of 11.01% and a mass fraction of lithium bromide of 33.37% was obtained, named as sample No. 2, and the yield of methyllithium was 99.0%.

Embodiment 3

[0039]Under normal pressure at 20-40°C, under the protection of inert gas argon, 14g metal lithium sand is quickly added to reactor 1 under the protection of 140g diethoxymethane, keep reactor 1 airtight, and add 95g methyl bromide to reactor 1 within 1 hour , the reactor is cooled with a low-temperature refrigerant interlayer, and the temperature is controlled at 20-40°C. After the mixture is added, it is kept at 30-40°C for 2 hours to obtain a solution; at the same time, 7g of metal lithium sand is quickly added to the reaction with 140g of diethoxymethane. In the reactor 2, keep the reactor 2 airtight, add 25g of methyl chloride to the reactor 2 in 1 hour, cool the reactor with a low-temperature refrigerant interlayer, control the temperature at 20-40°C, and keep the temperature at 30-40°C for 2 hours after the addition of the mixture is completed. Obtain B solution; Filter A solution, B solution respectively, mix according to A solution: B solution=1: 1, obtain methyl lithi...

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Abstract

The invention belongs to the technical field of chemical industrial and provides a stable methyllithium solution and a preparation method thereof. The methyllithium solution comprises, in percentage by mass, 3%-12% of methyllithium, 7%-35% of halide salt and the balance of a solvent, wherein the halide salt is at least one of chlorine salt, bromine salt and iodate salt, and the solvent adopts diethoxymethane. The finally prepared methyllithiume solution is more stable due to the fact that the halide salt is added to serve as a stabilizer, and a test shows that the decomposition rate is under 0.01 in 21 days and is remarkably reduced by comparison with a traditional methyllithium solution. The invention further provides the preparation method of the methyllithium solution, the reaction yield of the method is higher, waste in the production process is reduced, and the cost of methyllithium is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a stable methyllithium solution and a preparation method of the methyllithium solution. Background technique [0002] Organolithium compounds such as butyllithium are obtained by reacting lithium or a mixture of lithium and sodium with alkyl halides in an inert organic solvent. Usually, methyllithium is obtained by reacting methyl chloride with lithium metal to obtain the product and lithium chloride. [0003] CH 3 Cl+2Li→CH 3 Li+LiCl [0004] Usually, alkyllithiums such as butyllithium, sec-butyllithium and tert-butyllithium are synthesized in hydrocarbon solvents such as hexane and cyclohexane, while methyllithium is different from the above other alkyllithiums because of its presence in hydrocarbons It is insoluble in similar solvents, and is generally synthesized in solvents such as ether and tetrahydrofuran. Ethyl ether has serious safety hazards such as fire and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/02
Inventor 周卫强蒋国群储鹏史先乔
Owner JIANGSU CHANGJILI NEW ENERGY TECH CO LTD
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