RU94025036A - Method for producing normal butyl lithium - Google Patents

Method for producing normal butyl lithium

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Publication number
RU94025036A
RU94025036A RU94025036/04A RU94025036A RU94025036A RU 94025036 A RU94025036 A RU 94025036A RU 94025036/04 A RU94025036/04 A RU 94025036/04A RU 94025036 A RU94025036 A RU 94025036A RU 94025036 A RU94025036 A RU 94025036A
Authority
RU
Russia
Prior art keywords
lithium
synthesis
normal butyl
butyl chloride
production
Prior art date
Application number
RU94025036/04A
Other languages
Russian (ru)
Other versions
RU2095362C1 (en
Inventor
Г.Т. Щербань
Г.З. Сахапов
Ю.И. Рязанов
Л.М. Курочкин
Н.Р. Гильмутдинов
Г.В. Баев
Original Assignee
Г.Т. Щербань
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Г.Т. Щербань filed Critical Г.Т. Щербань
Priority to RU94025036A priority Critical patent/RU2095362C1/en
Publication of RU94025036A publication Critical patent/RU94025036A/en
Application granted granted Critical
Publication of RU2095362C1 publication Critical patent/RU2095362C1/en

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Abstract

FIELD: organic synthesis. SUBSTANCE: proposed method is carried out in two steps, in hydrocarbon solvent medium, by reacting normal butyl chloride with dispersed lithium metal. First process step is carried out at temperature 0-60 C, and second step is followed by curing reaction mass at 65-90 C. Normal butyl lithium is synthesized in first process step at molar ratio normal butyl chloride-to-lithium equal to 0.65-0.85 of stoichiometrically required ratio. Resulting reaction products are separated. Unreacted lithium is recycled back to synthesis conducted at same molar ratio of components. Resulting butyl lithium solution isolated by separation is directed to second synthesis step which is completed by adding portion of butyl lithium solution and remaining quantity of butyl chloride. Synthesis during first process step is effected by continuous circulation of reactions mass through cooler. Normal butyl chloride is metered out with mass velocity of (0.25-2.5) h* in relation to lithium and introduced into reactor, preferably, at point having lowest temperature. Method can be used for production of lithium organic compounds, in particular alkyl lithium ones used as monomer polymerization initiators in production of rubbers and thermoelastoplastics. EFFECT: cheaper and simpler method for synthesis of lithium organic compounds.

Claims (1)

Изобретение относится к получению литийорганических соединений, в частности алкиллитиевых, используемых в качестве инициаторов полимеризации мономеров в производствах каучуков и термоэластопластов. Предлагаемый способ получения бутиллития, осуществляемый в две стадии в среде углеводородного растворителя взаимодействием нормального хлористого бутила с дисперсией металлического лития при температуре 0 - 60oС в первой и во второй стадиях с последующей выдержкой реакционной массы при 65 - 90oC, основан на синтезе нормального бутиллития в первой стадии при мольном соотношении нормальный хлористый бутил: литий, равном 0,65 - 0,85 от стехиометрически необходимого, полученные продукты реакции подвергают сепарации, непрореагировавший литий подают вновь на синтез при том же соотношении компонентов, отделенный при сепарации раствор полученного бутиллития направляют на вторую стадию синтеза, которую завершают после добавления второй части раствора бутиллития и оставшегося количества нормального бутила хлористого, причем синтез в первой стадии осуществляют при непрерывной циркуляции реакционной массы через холодильник и нормальный бутил хлористый дозируют по отношению к литию с массовой скоростью 0,25 - 2,5 ч-1 и вводят, предпочтительно, в точку с наименьшей температурой.The invention relates to the production of organolithium compounds, in particular alkyl lithium compounds, used as initiators for the polymerization of monomers in the production of rubbers and thermoplastic elastomers. The proposed method for producing butyllithium, carried out in two stages in a hydrocarbon solvent, by the interaction of normal butyl chloride with a dispersion of lithium metal at a temperature of 0-60 o C in the first and second stages, followed by exposure of the reaction mass at 65 - 90 o C, based on the synthesis of normal butyl lithium in the first stage with a molar ratio of normal butyl chloride: lithium equal to 0.65 - 0.85 of the stoichiometrically necessary, the obtained reaction products are subjected to separation, unreacted lithium under The synthesis of the butyl lithium solution separated during separation is sent to the second synthesis stage, which is completed after the second part of the butyl lithium solution and the remaining amount of normal butyl chloride are added, the synthesis in the first stage being carried out by continuous circulation of the reaction mixture through a refrigerator and normal butyl chloride is dosed with respect to lithium at a mass rate of 0.25-2.5 h -1 and is introduced, preferably, at the point with the lowest temperature.
RU94025036A 1994-07-04 1994-07-04 Method of synthesis of normal butyllithium RU2095362C1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
RU94025036A RU2095362C1 (en) 1994-07-04 1994-07-04 Method of synthesis of normal butyllithium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
RU94025036A RU2095362C1 (en) 1994-07-04 1994-07-04 Method of synthesis of normal butyllithium

Publications (2)

Publication Number Publication Date
RU94025036A true RU94025036A (en) 1997-05-27
RU2095362C1 RU2095362C1 (en) 1997-11-10

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Family Applications (1)

Application Number Title Priority Date Filing Date
RU94025036A RU2095362C1 (en) 1994-07-04 1994-07-04 Method of synthesis of normal butyllithium

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RU (1) RU2095362C1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2691649C1 (en) * 2019-02-01 2019-06-17 Владимир Стефанович Глуховской Method of producing alkyl lithium

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Publication number Publication date
RU2095362C1 (en) 1997-11-10

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