CN101362772A - Method for preparing dibutylmagnesium - Google Patents

Method for preparing dibutylmagnesium Download PDF

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CN101362772A
CN101362772A CN 200810196897 CN200810196897A CN101362772A CN 101362772 A CN101362772 A CN 101362772A CN 200810196897 CN200810196897 CN 200810196897 CN 200810196897 A CN200810196897 A CN 200810196897A CN 101362772 A CN101362772 A CN 101362772A
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reaction
chlorobutane
solution
magnesium
solvent
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CN 200810196897
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Chinese (zh)
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丁墩墩
旋 刘
吴元欣
吴广文
炜 孙
刚 宋
张春桂
朱少坤
峻 杨
陶凌云
黄艳刚
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武汉工程大学
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Abstract

The invention relates to a preparation method for synthesizing dibutyl magnesium by taking 2-chlorobutane, magnesium powder and n-butyl lithium as raw materials. The 2-chlorobutane, the magnesium powder and the n-butyl lithium are taken as raw materials, and the dibutyl magnesium is synthesized under the condition of no water and no oxygenated solvent; the reaction process comprises: under the protection of N2, the magnesium powder is mixed with an evocating agent, then the mixture is put in a reaction kettle for heating and stirring and is added with a small amount of 2-chlorobutane solution slowly; after evocating reaction, under the condition of thermal insulation, the 2-chlorobutane solution is added into the reaction kettle slowly to generate a Grignard reagent by reaction; cooling and temperature reduction are carried out, n-butyl lithium hexane solution is added rapidly; after the reaction under the condition of thermal insulation is carried out, a solvent is obtained by distilling and separating; cooling and filtering are carried out, thus obtaining the dibutyl magnesium; in the preparation process, the mixture ratio of each raw material is as follows: the mole ratio of the magnesium powder to 2-chlorobutane to n-butyl lithium is equal to 1.0-1.2: 1: 1. The preparation method has the advantages of simple and easy technique, no pollution, being investment-saving, high magnesium powder conversion rate and product yield, etc.

Description

二丁基镁的制备方法 Preparation of dibutylmagnesium

技术领域 FIELD

本发明涉及一种以2-氯丁垸、镁粉、正丁基锂为原料合成二丁基镁的制备方法。 The present invention relates to a embankment 2- chlorobutanol, magnesium, n-butyllithium is prepared synthesized dibutylmagnesium. 背景技术 Background technique

有机卤化镁即格氏试剂在化学反应中有很广泛的应用。 Organomagnesium halide with a Grignard reagent that is very widely used in chemical reactions. 同格氏试剂相比,二烷基镁反应同有机卤化镁类似而应用要少得多。 Compared with a Grignard reagent, dialkylmagnesium analogous reaction with an organic magnesium halide and the application is much less. 其主要原因是至今为止还没有合适的方法大量生产二烷基镁。 The main reason is so far no suitable method for mass production of a dialkyl magnesium. 二烷基镁与格氏试剂及烷基锂相比具有原料成本低、运输容易。 Dialkyl magnesium with an alkyl lithium and a Grignard reagent compared to low raw material cost, easy to transport. 特别是二烷基镁具有优良的化学性能,与烷基锂相比二烷基镁具有更好的热稳定性和弱的引燃性(醚溶液)。 In particular dialkyl magnesium having excellent chemical properties, thermal stability and better ignitability weak (ether solution) compared to the dialkyl magnesium with an alkyl lithium. 二烷基镁甚至可用于烷基锂烃溶液的稳定剂。 Dialkylmagnesium even be used for the alkylation of a hydrocarbon solution of lithium stabilizing agent. 与有机卤化镁相比,二烷基镁在烃类溶剂中稳定性更强,反应产率更高。 Compared with the organomagnesium halide, dialkylmagnesium greater stability in a hydrocarbon solvent, a higher reaction yield. 二烷基镁类似于烷基锂,可作为有机化合物的金属化试剂,如苯、甲苯等,还可以同不饱和有机化合物反应。 Dialkyl magnesium like alkyllithium reagents can be used as the metal organic compound, such as benzene, toluene and the like, it may also be the reaction with the unsaturated organic compound.

二丁基镁,英文名称:Dibutylmagnesium (简称DBM),有多种同分异构体。 Dibutylmagnesium, English name: Dibutylmagnesium (referred to as the DBM), a variety of isomers. 溶于醚类, 纯的二丁基镁为不挥发的固体,但由于其固体极易燃,所以成品制成14%的己烷溶液或17 %的庚烷溶液。 Was dissolved in ether, dibutyl magnesium is pure non-volatile solids, but because of its extremely flammable solids, it is made 14% or 17% hexanes in heptane finished.

二丁基镁由于在制备方法上的缺陷一直没有格氏试剂那样广泛应用。 Dibutylmagnesium due to a defect in the production method has not been widely used as Grignard reagent. 最早的制备方法是由垸基汞被镁粉还原而得,其反应如下: R2Hg+Mg— R2Mg+Hg The first is prepared by reduction of magnesium alkyl with mercury is obtained, the reaction is as follows: R2Hg + Mg- R2Mg + Hg

这个制备过程受到了汞的髙额价位及其使用时对人体的伤害两方面所限制。 Bodily harm both the restrictions on the preparation process has been priced Gao amount of mercury and its use. 事实上一般情况 In fact general

下,垸基汞就是由镁制得。 Next, alkyl with mercury is obtained by the magnesium. 这个反应一般要在碱性环境中进行,与其在格氏试剂综合反应中 This reaction is generally carried out in an alkaline environment, rather than the Grignard reagent synthesis reaction

必须要在无碱的环境下进行相比,它会分解更多的垸基镁。 Must be carried out than in the alkali-free environment, it will decompose more alkyl with magnesium.

其次通过加入二噁烷使其与卤化镁以络合物的形式析出,反应如下: Then precipitated as a complex by the addition of dioxane was reacted with a magnesium halide, the reaction is as follows:

2RMgX+C4H80" R2Mg+ C4H802.MgX2 2RMgX + C4H80 "R2Mg + C4H802.MgX2

因为二噁垸本身呈碱性使得此反应不可能在无碱环境下完成,因此,由于二丁基镁制备困难, Because dioxane was embankment itself so that the basic reaction is impossible at this alkali environment, therefore, difficult since the preparation of dibutylmagnesium,

具有汞污染和必须在碱性环境下完成,使其生产受到极大的限制。 Having mercury and must be done in an alkaline environment, their production is greatly limited. 发明内容 SUMMARY

本发明所要解决的技术问题是针对上述现有技术存在的不足而提供了一种二丁基镁制备方法,它具有工艺简单易行、无污染、成本低、镁粉转化率和产品收率高的优点。 The present invention solves the technical problem for the shortcomings of the prior art described above and provide a method for preparing dibutyl magnesium, which has simple and easy process, pollution, low cost, and the conversion of magnesium product yield The advantages. 本发明为解决上述提出的问题所釆用的的技术方案为: The present invention is made to solve the above problems preclude the use of the technical solution is:

以2-氯丁烷、镁粉、正丁基锂为原料,在无水、无氧溶剂条件下合成二丁基镁,其反应 2-chlorobutane, magnesium, n-butyllithium was synthesized dibutylmagnesium under anhydrous, anaerobic conditions of the solvent, the reaction

过程包括:在Na保护下,将镁粉、引发剂混合,置于反应釜中加热、搅拌,并缓慢加入少量 The process comprising: Under protection Na, magnesium powder, mixing agents initiator, placed in the reaction kettle was heated, with stirring, was slowly added a small amount of

2-氯丁垸溶液,引发反应后,在保温情况下,将2-氣丁烷溶液缓慢加入反应釜,反应生成格氏试剂CH,CH3CH(CH,)MgCl;冷却降温,快速加入正丁基锂正己烷溶液,保温反应后,蒸馏分离出溶剂,冷却过滤,制备得到二丁基镁:制备过程中各原料的配比为:镁粉:2-氯丁烷: 2- chlorobutanol embankment solution, after the reaction initiation, incubation in the case where, 2- butane gas was slowly added to the kettle, the reaction of a Grignard reagent CH, CH3CH (CH,) MgCl; cool down rapidly added n-butyl lithium n-hexane solution, after the incubation the reaction, the solvent was separated by distillation, cooled and filtered, dibutylmagnesium prepared: preparation process for the proportion of the raw materials: magnesium: 2-chlorobutane:

正丁基锂的摩尔比为1.0〜1.2 : i: l。 The molar ratio of n-butyllithium was 1.0~1.2: i: l.

按上述方案,所述的引发剂为I,、 Br2、碘甲烷、溴甲烷或格氏试剂:所述引发剂的加入量按重量计为2-教丁垸所用量的0.1~0. 5%。 The above-described embodiment, the initiator is I ,, Br2, methyl iodide, methyl bromide, or a Grignard reagent: the initiator agent is added in an amount by weight of 2-butoxy embankment teach the amount of 0.1 to 05%.

按上述方案,所述的反应釜为带有搅拌、回流冷凝器、氮气导入管、滴液漏斗的反应釜内,反应过程通入氮气。 The above-described embodiment, the reaction vessel was equipped with a stirring, a reflux condenser, a nitrogen gas introducing tube, a dropping funnel reactor, purged with nitrogen during the reaction.

按上述方案,在反应引发后,将2-氯丁烷溶液缓慢滴加至反应釜内,反应温度控制在30 •C〜100"C;滴加完毕后,继续搅拌,保温反应1.5〜3小时。 According to the above embodiment, after the reaction initiation, 2-chlorobutane solution was slowly added dropwise to the reaction vessel, the reaction temperature was controlled at 30 • C~100 "C; After the addition was complete, stirring was continued, the reaction 1.5~3 hr incubation .

按上述方案,在生成格氏试剂后,冷却降温,在0"〜60X:温度下,快速加入正丁基锂正己烷溶液,保温反应1〜2小时,保温温度控制在30"C〜120"C。 According to the above embodiment, after generating the Grignard reagent, cool down, at 0 "~60X: temperature, rapid n-hexane solution of n-butyllithium was added, the reaction incubated ~ 2 hours, incubation temperature controlled at 30" C~120 " C.

按上述方案,所述的2-铽丁烷溶液由2-氣丁烷与溶剂配制而成,溶液浓度为0.6〜 1.05mol/L ,所述的溶剂为乙醚,或为四氢呋喃、苯、甲苯、正己烷中的任意一种。 According to the above embodiment, the 2-terbium solution prepared from 2-butane and butane gas from a solvent, solution concentration of 0.6~ 1.05mol / L, the solvent is diethyl ether or tetrahydrofuran, benzene, toluene, any one of n-hexane.

按上述方案,所述的正丁基锂正己烷溶液由正丁基锂与溶剂正己烷配制而成,溶液的摩尔浓度为2. 5mol/L。 According to the above embodiment, the n-butyl lithium n-hexane solution prepared from n-butyllithium and n-hexane from the solvent, the molar concentration of the solution was 2. 5mol / L.

按上述方案,蒸馏分离出溶剂,静置后取上层清液;将少量金属锂剪成小片加入上述上清液中,缓慢搅拌,充氣气保护,滤出未反应的金属锂,用络合滴定法分析二丁基镁的浓度, 加入正己烷,配成一定浓度的二丁基镁溶液。 The above-described embodiment, the solvent is separated by distillation, taking supernatant after standing; a small amount of metal lithium into small pieces was added to the supernatant, slowly stirring, inflatable protective gas, the unreacted lithium metal was filtered off using complexometric titration method of analysis of concentration of dibutylmagnesium, n-hexane, dubbed a certain concentration of solution of dibutyl magnesium. 收集的溶剂可循环使用。 The solvent collected can be recycled.

上述反应中反应釜内搅拌速度为100〜700转/分;反应釜内要求无水、无氧,并充氮气保护。 Stirring rate in the above reaction kettle was 100~700 revolutions / min; reaction kettle claim dehydrated and deoxygenated and flushed with nitrogen.

本发明的反应式为: The reaction of the present invention is of formula:

CHaCHiCH(CH3) Cl + Mg——CHaCH^lKOUMgCl CH復CH咖MgCl + CH潔HiCH山i——CH潔H卿g (CH,) CHCH2CH3 CC,,) Cl + 2 Li——CCH(CH,) Li + LiCl CH、CCH,) Li + CH线CH(CH》MgCl——[CH馬H(Ol,) ]2Mg + LiCl 格氏试剂合成的引发比较缓慢,应在加热和缓慢搅拌的条件下进行。反应引发后,反应比较迅速,并伴随有大量的反应热,易发生如下副反应: CHaCHiCH (CH3) Cl + Mg - CHaCH ^ lKOUMgCl CH CH coffee complex MgCl + CH cleaning HiCH Hill i - CH H Jie Qing g (CH,) CHCH2CH3 CC ,,) Cl + 2 Li - CCH (CH,) li + LiCl CH, CCH,) li + CH lines CH (CH "MgCl - [CH Ma H (Ol,)] 2Mg + LiCl Grignard reagent synthesized relatively slow initiator, and heating should be carried out under slow stirring conditions after the reaction initiator to react relatively quickly, and is accompanied by a large amount of reaction heat, the following side effects likely to occur:

OW^CfKCfQ Cl + 2Mg——CHaCH^CH(CH,) CH(CK,) CHzCH, + MgCl2 解决的办法有:(1)降温,使用的反应釜应配备冷却换热装置,加快搅拌,使反应混合物均匀混合,避免局部过热,确保反应有效进行。 OW ^ CfKCfQ Cl + 2Mg - CHaCH ^ CH (CH,) CH (CK,) CHzCH, + MgCl2 solution has: (1) cooling, the reaction vessel should be equipped with cooling using heat exchange means, to speed up the stirring, the reaction the mixture was uniformly mixed to avoid local overheating, to ensure that the reaction effectively. (2)将2-氯丁烷与溶剂乙醚混合配制成低浓度 (2) 2-chloro-butane with a solvent mixture of diethyl ether formulated as a low concentration

的溶液,缓慢加入到反应釜内,控制反应速率。 It was slowly added into the reactor, controlling the reaction rate.

格氏试剂与丁基锂反应生成二丁基镁的反应非常迅速,而且反应非常完全。 Generating dibutyl magnesium Grignard reagent is reacted with butyl lithium reaction is very rapid, and the reaction is complete. 为了增大LiCl 颗粒的粒径,易于分离,需要降低反应温度和搅拌速度。 In order to increase the particle diameter of LiCl, easy to separate, it is necessary to reduce the reaction temperature and stirring rate. 分离出来的LiCl可以回收利用,降低生产成本,有利环境保护。 LiCl separated can be recycled, reduce production costs, favorable environmental protection.

本发明的有益效果在于:1、采用两歩法完成制备过程,制备过程简便有效;2、制备成本低,无污染,有利环境保护;3、镁粉转化率和产品收率髙,且收集的溶剂可循环使用。 Advantageous effects of the present invention is: 1, to complete the preparation process using two ho method, simple and effective preparation process; 2, low preparation cost, pollution, environmental protection is advantageous; 3, the conversion rate and the product yield magnesium Gao, and collected The solvent can be recycled. 具体实施方式 detailed description

以下通过实施例进一歩具体说明本发明。 The following examples ho into a detailed description of the present invention.

实施例l: Example l:

向装有搅拌器、滴液漏斗、温度计、氮气导入管,回流冷凝器(上装干燥管)的250ml 四口烧瓶反应器中通入氮气,加热驱除水蒸气,达到IOOIC后移去热源。 Equipped with a stirrer, a dropping funnel, a thermometer, a nitrogen gas introducing tube, 250ml four-neck flask reactor with a reflux condenser (tops drying tube) was purged with nitrogen, purge the steam heating, the heat source was removed after reaching IOOIC. 待温度降到约7(TC 时,加入3.65g(0.15mol)镁粉、2g2-氯丁垸、30mL乙醚和一粒碘,缓慢搅拌,使反应釜中物料稳定回流10〜20分钟,控制温度在34C左右。反应器中液体变为棕色,待红棕色褪去后,开始缓慢滴加2-氯丁烷溶液,2-氯丁烷溶液由15g2-氯丁烷和llOraL乙醚混合而成;控制反应温度在33"〜35",滴加完毕后,继续搅拌反应3小时,然后向反应器中快速加入60mL 含有2.5mol/L正丁基锂的JE己烷溶液,降低搅拌速度,控制反应温度为0C〜5X:。反应完毕过滤分离,滤液用EDTA (络合滴定法)分析Mg含量,计算得产品收率为85%。 When the temperature dropped to about 7 (TC, was added 3.65g (0.15mol) of magnesium powder, 2 g of 2 chlorobutanol embankment, an iodine and 30 mL of diethyl ether, stirred slowly, the reaction mass in the autoclave stabilized at reflux for 10-20 minutes, the temperature control in the liquid reactor, about 34C to brown, reddish brown fade until, slowly added dropwise a solution of 2-chloro-butane, 2-chlorobutane solution was mixed by a 15g2- chlorobutane and llOraL from diethyl ether; control reaction temperature 33 "~ 35", after the addition was complete, stirring was continued for 3 hours, then quickly added a hexane solution containing JE 60mL 2.5mol / L n-butyl lithium to the reactor, the stirring speed is reduced, the reaction temperature is controlled 0C~5X :. After the reaction was separated by filtration, the filtrate Mg content analyzed by EDTA (complexometric titration), calculated to give the product in 85% yield.

实施例2: Example 2:

向装有搅拌器、滴液漏斗、温度计、氮气导入管,回流冷凝器(上装干燥管)的250ml 四口烧瓶反应器中通入氮气,加热驱除水蒸气,达到IO(TC后移去热源。待温度降到约7(TC 时,加入3.65 g( 0.15mol)镁粉、2g2-氯丁烷、30mL正己垸和一粒碘,缓慢搅拌,控制温度在65C左右。瓶内液体变为玫瑰红色,待玫瑰红色褪去,缓慢滴加2-氯丁垸溶液,2-氯丁烷溶液由15g2-氯丁烷和U0raL正己垸混合而成;反应温度控制在60"〜68",继续搅拌反应3小时,然后向反应器中快速加入60mL含有2.5mol/L正丁基锂的正己烷溶液,降低搅拌速度,控制反应温度为0C〜5X:。反应完毕过滤分离,滤液用EDTA分析Mg含量,计算得产品收率为75%。 Equipped with a stirrer, a dropping funnel, a thermometer, a nitrogen gas introducing tube, 250ml four-neck flask reactor with a reflux condenser (tops drying tube) was purged with nitrogen, heated purge steam reaches IO (TC after the heat source is removed. the temperature dropped to about 7 (TC, the addition of 3.65 g (0.15mol) of magnesium powder, 2 g of 2-chlorobutane, 30 mL n-hexyl iodide embankment and a slowly stirring, controlling the temperature at about 65C. bottle of liquid to a rose color to be faded red rose was slowly added dropwise a solution of 2- chlorobutanol embankment, by mixing a solution of 2-chloro-butane-chlorobutane and U0raL 15g2- embankment from n-hexyl; the reaction temperature was controlled at 60 "~68", the reaction was stirred 3 hours, and then quickly added 60mL n-hexane solution containing 2.5mol / L n-butyl lithium to the reactor, the stirring speed is reduced, the reaction temperature is controlled 0C~5X :. After the reaction was separated by filtration, the filtrate was analyzed with EDTA Mg content, calculated to obtain the product in 75% yield.

实施例3: Example 3:

向装有搅拌器、滴液漏斗、温度计、氮气导入管,回流冷凝器(上装干燥管)的250ml 四口烧瓶反应器中通入氮气,加热驱除水蒸气,达到IOO"C后移去热源。待温度降到约70X: 时,加入4.4 g (0.18mol)镁粉、3g2-氯丁烷、lOOmL乙醚和碘,缓慢搅拌,控制温度在33 'C左右。瓶内液体变为红棕色,待红棕色褪去,缓慢滴加2-氯丁烷溶液,2-氯丁烷溶液由14g2- Equipped with a stirrer, a dropping funnel, a thermometer, a nitrogen gas introducing tube, 250ml four-neck flask reactor with a reflux condenser (tops drying tube) was purged with nitrogen, purge steam heating, to achieve IOO "C after the heat source is removed. the temperature dropped to about 70X: when added 4.4 g (0.18mol) magnesium, 3g2- chlorobutane, diethyl ether and iodine lOOmL stirred slowly, controlling the temperature at about 33 'C to reddish brown bottle of liquid to be. faded red-brown, solution was slowly added dropwise 2-chlorobutane, 2-chlorobutane solution consisting 14g2-

氯丁垸和160mL乙醚混合而成。 Chlorobutanol embankment and 160mL ether mixture. 反应温度控制在331C〜351C,继续搅拌反应3小时,然后向反应器中快速加入60mL含有2.5mol/L正丁基锂的正己烷溶液,降低搅拌速度,控制反应温度为0TC〜5"C。反应完毕过滤分离,滤液用EDTA分析Mg含量,计算得产品收率为76%。 实施例4: The reaction temperature is controlled at 331C~351C, stirring was continued for 3 hours, then quickly added 60mL n-hexane solution containing 2.5mol / L n-butyl lithium to the reactor, the stirring speed is reduced, the reaction temperature is controlled 0TC~5 "C. The mixture was then separated by filtration, the filtrate was analyzed with EDTA Mg content, calculated yield was 76% Example 4:

向装有搅拌器、滴液漏斗、温度计、贫气导入管,回流冷凝器(上装干燥管)的250ml 四口烧瓶反应器中通入徵气,加热驱除水蒸气,达到1001C后移去热源。 Equipped with a stirrer, a dropping funnel, a thermometer, a lean gas inlet tube, a reflux condenser (with a drying tube tops) in 250ml four-neck flask reactor into intrinsic gas, purge steam heating, the heat source was removed after reaching 1001C. 待温度降到约70"C 时,加入4.9 g (0.2raol)镁粉、2g2-氯丁烷、30mL正己烷和一粒碘,缓慢搅拌,控制温度在65X:左右。瓶内液体变为玫瑰红色,待玫瑰红色褪去,缓慢滴加2-叛丁烷溶液,2-叛丁烷溶液由15g2-氯丁垸和110mL正己烷混合而成:反应温度控制在601C〜68TC,继续搅拌反应3小时,然后向反应器中快速加入601111含有2.511101/1正丁基锂的正己烷溶液,降低搅拌速度,控制反应温度为0X:〜51C。反应完毕过滤分离,滤液用EDTA分析Mg含量,计算得产品收率为76.6%。 When the temperature dropped to about 70 "C, was added 4.9 g (0.2raol) magnesium powder, 2 g of 2-chlorobutane, 30 mL of n-hexane and an iodine slow stirring, temperature control in 65X:. Bottle of liquid to about Rose red, rose red be faded, was slowly added dropwise a solution of 2- betray butane, 2-butane betrayed by mixing a solution of 110mL of n-hexane and the embankment 15g2- chloroprene from: controlling the reaction temperature 601C~68TC, the reaction was continued for 3 hours , then quickly added to the reactor containing 601 111 2.511101 / n-hexane solution of n-butyllithium, reduced stirring speed, reaction temperature is controlled 0X:. ~51C After the reaction was separated by filtration, the filtrate was analyzed with EDTA Mg content, calculated product The yield was 76.6%.

Claims (7)

  1. 1、一种二丁基镁的制备方法,其特征在于:以2-氯丁烷、镁粉、正丁基锂为原料,在无水、无氧溶剂条件下合成二丁基镁,其反应过程包括:在N2保护下,将镁粉、引发剂混合,置于反应釜中加热、搅拌,并缓慢加入少量2-氯丁烷溶液,引发反应后,在保温情况下,将2-氯丁烷溶液缓慢加入反应釜,反应生成格氏试剂CH3CH2CH(CH3)MgCl;冷却降温,快速加入正丁基锂正己烷溶液,保温反应后,蒸馏分离出溶剂,冷却过滤,制备得到二丁基镁;制备过程中各原料的配比为:镁粉∶2-氯丁烷∶正丁基锂的摩尔比为1.0~1.2∶1∶1。 1, a process for preparing dibutylmagnesium, wherein: 2-chlorobutane, magnesium, n-butyllithium was synthesized dibutylmagnesium under anhydrous, anaerobic conditions of the solvent, the reaction the process comprising: under N2 protection, magnesium powder, mixing agents initiator, placed in the reaction kettle was heated, with stirring, was slowly added a small amount of a solution of 2-chloro-butane, the reaction was initiated, in the case of incubation, chlorobutanol 2- dioxane solution was slowly added to the kettle, the reaction of a Grignard reagent CH3CH2CH (CH3) MgCl; cool down rapidly n-butyllithium n-hexane solution was added. after incubation the reaction, the solvent was separated by distillation, cooled and filtered, prepared dibutyl magnesium; the preparation process is the ratio of the raw materials: magnesium :2--chlorobutane: n-butyllithium molar ratio of 1.0 to 1.2:1:1.
  2. 2、 按权利要求1所述二丁基镁的制备方法,其特征在于所述的引发剂为L、 Br2、碘甲垸、溴甲烷或格氏试剂;所述引发剂的加入量按重量计为2_氯丁烷所用量的0.1〜0.5%。 2, prepared according to claim 1 said method butylmagnesium two claims, wherein the initiator is L, Br2, embankment methyl iodide, methyl bromide or Grignard reagent; the initiator agent is added in an amount by weight 2_ chlorobutane 0.1~0.5% of the amount. .
  3. 3、 按权利要求1所述二丁基镁的制备方法,其特征在于所述的反应釜为带有搅拌、回流冷凝器、氮气导入管、滴液漏斗的反应釜内,反应过程通入氮气。 3, prepared according to claim 1 said method butylmagnesium two claims, characterized in that said reaction vessel is equipped with a stirring, a reflux condenser, a nitrogen gas introducing tube, a dropping funnel reactor, the reaction flushed with nitrogen .
  4. 4、 按权利要求1所述二丁基镁的制备方法,其特征在于在反应引发后,将2-氯丁烷溶液缓慢滴加至反应釜内,反应温度控制在3ox:〜ioox:;滴加完毕后,继续搅拌,保温反应1. 5〜3小时。 4, prepared according to claim 1 said method butylmagnesium two claims, characterized in that after the reaction initiation, 2-chlorobutane solution was slowly added dropwise to the reaction vessel, the reaction temperature is controlled at 3ox: ~ioox :; drops after the addition is completed, stirring was continued, the reaction incubated 1. 5~3 hours.
  5. 5、 按权利要求1所述二丁基镁的制备方法,其特征在于在生成格氏试剂后,冷却降温, 在0"〜601C温度下,快速加入正丁基锂正己烷溶液,保温反应1〜2小时,保温温度控制在30"C〜120X:。 5, prepared according to claim 1 said method butylmagnesium two claims, characterized in that after generating a Grignard reagent, cool down, at 0 "~601C temperature rapidly n-butyllithium n-hexane solution was added, the reaction incubated 1 ~ 2 hours, incubation temperature controlled at 30 "C~120X :.
  6. 6、 按权利要求1所述二丁基镁的制备方法,其特征在于所述的2-氯丁烷溶液由2-氯丁烷与溶剂配制而成,溶液浓度为0.6〜1.05mol/L,所述的溶剂为乙醚,或为四氢呋喃、苯、 甲苯、正己垸中的任意一种。 6, according to claim 1 of the production method of dibutylmagnesium, characterized in that the 2-chlorobutane was prepared from 2-chlorobutane obtained by solvent, concentration of the solution 0.6~1.05mol / L, the solvent is diethyl ether or tetrahydrofuran, benzene, toluene, n-hexyl any one of the embankment.
  7. 7、 按权利要求1所述二丁基镁的制备方法,其特征在于所述的正丁基锂正己垸溶液由正丁基锂与溶剂正己烷配制而成,溶液的摩尔浓度为2. 5mol/L。 7. The process as claimed in claim 1 of dibutylmagnesium, wherein said n-hexyl n-butyl lithium solution was prepared by the embankment with a solvent of n-butyllithium n-hexane from the molar concentration of the solution was 2. 5mol / L.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9499880B2 (en) * 2015-03-06 2016-11-22 Battelle Memorial Institute System and process for production of magnesium metal and magnesium hydride from magnesium-containing salts and brines

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9499880B2 (en) * 2015-03-06 2016-11-22 Battelle Memorial Institute System and process for production of magnesium metal and magnesium hydride from magnesium-containing salts and brines

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