CN101362772A - The preparation method of dibutylmagnesium - Google Patents
The preparation method of dibutylmagnesium Download PDFInfo
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- CN101362772A CN101362772A CNA2008101968974A CN200810196897A CN101362772A CN 101362772 A CN101362772 A CN 101362772A CN A2008101968974 A CNA2008101968974 A CN A2008101968974A CN 200810196897 A CN200810196897 A CN 200810196897A CN 101362772 A CN101362772 A CN 101362772A
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- KJJBSBKRXUVBMX-UHFFFAOYSA-N magnesium;butane Chemical compound [Mg+2].CCC[CH2-].CCC[CH2-] KJJBSBKRXUVBMX-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims abstract description 32
- BSPCSKHALVHRSR-UHFFFAOYSA-N 2-chlorobutane Chemical compound CCC(C)Cl BSPCSKHALVHRSR-UHFFFAOYSA-N 0.000 claims abstract description 31
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 31
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000007818 Grignard reagent Substances 0.000 claims abstract description 13
- 150000004795 grignard reagents Chemical class 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- ANUZKYYBDVLEEI-UHFFFAOYSA-N butane;hexane;lithium Chemical compound [Li]CCCC.CCCCCC ANUZKYYBDVLEEI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
- 238000005194 fractionation Methods 0.000 claims description 3
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 claims description 2
- 125000001033 ether group Chemical group 0.000 claims description 2
- 230000000977 initiatory effect Effects 0.000 claims description 2
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract 2
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 description 23
- 229910052749 magnesium Inorganic materials 0.000 description 14
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- 241000220317 Rosa Species 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 230000026030 halogenation Effects 0.000 description 3
- 238000005658 halogenation reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- -1 alkyl magnesium Chemical compound 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- GVNVAWHJIKLAGL-UHFFFAOYSA-N 2-(cyclohexen-1-yl)cyclohexan-1-one Chemical compound O=C1CCCCC1C1=CCCCC1 GVNVAWHJIKLAGL-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 101150065749 Churc1 gene Proteins 0.000 description 1
- 102100038239 Protein Churchill Human genes 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
本发明涉及一种以2－氯丁烷、镁粉、正丁基锂为原料合成二丁基镁的制备方法。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；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。本发明具有工艺简单易行、无污染、投资省、镁粉转化率和产品收率高等优点。The invention relates to a preparation method for synthesizing dibutyl magnesium by using 2-chlorobutane, magnesium powder and n-butyl lithium as raw materials. Using 2-chlorobutane, magnesium powder, and n-butyllithium as raw materials, dibutylmagnesium is synthesized under anhydrous and oxygen-free solvent conditions. The reaction process includes: under the protection of N2 , magnesium powder and initiator are mixed , placed in the reaction kettle to heat and stir, and slowly add a small amount of 2-chlorobutane solution, after the reaction is initiated, slowly add the 2-chlorobutane solution to the reaction kettle under the condition of heat preservation, and the reaction generates Grignard reagent; cooling down , quickly add n-butyllithium n-hexane solution, after heat preservation reaction, distill and separate the solvent, cool and filter, and prepare dibutylmagnesium; the ratio of each raw material in the preparation process is: magnesium powder: 2-chlorobutane: n- The molar ratio of butyllithium is 1.0˜1.2:1:1. The invention has the advantages of simple and easy process, no pollution, low investment, high conversion rate of magnesium powder and high product yield.
Description
Technical field
The present invention relates to a kind of is the preparation method of the synthetic dibutylmagnesium of raw material with Sec-Butyl Chloride, magnesium powder, n-Butyl Lithium.
Background technology
Organic halogenation magnesium is that Grignard reagent has application very widely in chemical reaction.Tong Geshi reagent is compared, and dialkyl magnesium reaction is similar and use and want much less with organic halogenation magnesium.Its major cause is also not have suitable method mass production dialkyl magnesium up to now.Dialkyl magnesium compare with Grignard reagent and lithium alkylide have that raw materials cost is low, transportation easily.Particularly dialkyl magnesium has the excellent in chemical performance, compares dialkyl magnesium with lithium alkylide and has better thermostability and weak igniting property (ethereal solution).Dialkyl magnesium even can be used for the stablizer of lithium alkylide hydrocarbon solution.Compare with organic halogenation magnesium, dialkyl magnesium stability in varsol is stronger, and reaction yield is higher.Dialkyl magnesium is similar to lithium alkylide, can be used as the metallization reagent of organic compound, as benzene, toluene etc., can also react with unsaturated organic compound.
Dibutylmagnesium, English name: Dibutylmagnesium (being called for short DBM) has multiple isomers.Be dissolved in ethers, pure dibutylmagnesium is nonvolatile solid, but since its solid very easily fire, so finished product is made 14% hexane solution or 17% n-heptane solution.
Dibutylmagnesium is because the defective on the preparation method never has the such widespread use of Grignard reagent.Preparation method is the earliest reduced and gets by the magnesium powder by mercury alkylide, and its reaction is as follows:
R
2Hg+Mg→R
2Mg+Hg
This preparation process be subjected to the great number price of mercury and when using injury two aspects to human body limit.In fact generally speaking, mercury alkylide is made by magnesium exactly.This reaction generally will be carried out in alkaline environment, must compare under the environment of alkali-free in the Grignard reagent combined reaction with it, and it can decompose more alkyl magnesium.
Secondly by adding diox itself and magnesium halide are separated out with the form of complex compound, react as follows:
2RMgX+C
4H
8O
2→R
2Mg+C
4H
8O
2·MgX
2
Make this reaction under alkali free environment, not finish because diox itself is alkalescence, therefore,, make its production be subjected to great restriction because dibutylmagnesium preparation difficulty has mercury pollution and must finish under alkaline environment.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that exists at above-mentioned prior art and a kind of dibutylmagnesium preparation method is provided, it have simple for process, pollution-free, cost is low, magnesium powder transformation efficiency and the high advantage of product yield.
The present invention for the technical scheme that problem adopted of the above-mentioned proposition of solution is:
With Sec-Butyl Chloride, magnesium powder, n-Butyl Lithium is raw material, synthetic dibutylmagnesium under anhydrous, anaerobic solvent condition, and its reaction process comprises: at N
2Protection mixes magnesium powder, initiator down, places the reactor heating, stirs, and slowly add a small amount of Sec-Butyl Chloride solution, after the initiation reaction, under the insulation situation, Sec-Butyl Chloride solution is slowly added reactor, and reaction generates Grignard reagent CH
3CH
2CH (CH
3) MgCl; Cool, add the n-Butyl Lithium hexane solution fast, after the insulation reaction, fractionation by distillation goes out solvent, and cold filtration prepares dibutylmagnesium; Each proportion of raw materials is in the preparation process: magnesium powder: Sec-Butyl Chloride: the mol ratio of n-Butyl Lithium is 1.0～1.2: 1: 1.
Press such scheme, described initiator is I
2, Br
2, methyl iodide, monobromethane or Grignard reagent; The add-on of described initiator is 0.1～0.5% of Sec-Butyl Chloride institute consumption by weight.
Press such scheme, described reactor is to have in the reactor of stirring, reflux exchanger, nitrogen ingress pipe, dropping funnel, and reaction process feeds nitrogen.
Press such scheme, after reaction causes, Sec-Butyl Chloride solution is slowly dropped in the reactor, temperature of reaction is controlled at 30 ℃～100 ℃; After dropwising, continue to stir insulation reaction 1.5～3 hours.
Press such scheme, after generating Grignard reagent, cool, under 0 ℃～60 ℃ temperature, add the n-Butyl Lithium hexane solution fast, insulation reaction 1～2 hour, holding temperature are controlled at 30 ℃～120 ℃.
Press such scheme, described Sec-Butyl Chloride solution is formulated by Sec-Butyl Chloride and solvent, and strength of solution is 0.6～1.05mol/L, and described solvent is an ether, or is in tetrahydrofuran (THF), benzene, toluene, the normal hexane any one.
Press such scheme, described n-Butyl Lithium hexane solution is formulated by n-Butyl Lithium and solvent normal hexane, and the volumetric molar concentration of solution is 2.5mol/L.
Press such scheme, fractionation by distillation goes out solvent, gets supernatant liquid after leaving standstill; The little metal lithium is cut into small pieces adds in the above-mentioned supernatant liquor, slowly stir, the inflated with nitrogen protection leaches the unreacted metal lithium, and the concentration with complexometry analysis dibutylmagnesium adds normal hexane, is made into certain density dibutylmagnesium solution.The solvent of collecting can be recycled.
The interior stirring velocity of reactor is 100～700 rev/mins in the above-mentioned reaction; Require anhydrous, anaerobic in the reactor, and the inflated with nitrogen protection.
Reaction formula of the present invention is:
CH
3CH
2CH(CH
3)Cl+Mg——CH
3CH
2CH(CH
3)MgCl
CH
3CH
2CH(CH
3)MgCl+CH
3CH
2CH
2CH
2Li——CH
3CH
2CH
2CH
2Mg(CH
3)CHCH
2CH
3
CH
3CH
2CH(CH
3)Cl+2Li——CH
3CH
2CH(CH
3)Li+LiCl
CH
3CH
2CH(CH
3)Li+CH
3CH
2CH(CH
3)MgCl——[CH
3CH
2CH(CH
3)]
2Mg+LiCl
The Grignard reagent synthetic causes slower, should carry out under heating and slow stirring condition.Reaction is reacted rapider, and is attended by a large amount of reaction heat after causing, and following side reaction easily takes place:
CH
3CH
2CH(CH
3)Cl+2Mg——CH
3CH
2CH(CH
3)CH(CH
3)CH
2CH
3+MgCl
2
The way that solves has: (1) cooling, the reactor of use should be equipped with the cooling heat transferring device, accelerates to stir, and makes the reaction mixture uniform mixing, avoids local superheating, guarantees to react and effectively carries out.(2) Sec-Butyl Chloride and solvent ether are hybridly prepared into the solution of lower concentration, slowly join in the reactor control speed of reaction.
The reaction of Grignard reagent and butyllithium reaction generation dibutylmagnesium is very fast, and reaction is very complete.In order to increase the LiCl particle grain size, be easy to separate, need to reduce temperature of reaction and stirring velocity.The LiCl that separates can recycle, and reduces production costs the enabling environment protection.
Beneficial effect of the present invention is: 1, adopt two-step approach to finish preparation process, preparation process is simple and effective; 2, preparation cost is low, and is pollution-free, the enabling environment protection; 3, magnesium powder transformation efficiency and product yield height, and the solvent of collecting can be recycled.
Embodiment
Further specify the present invention by the following examples.
Embodiment 1:
To agitator, dropping funnel, thermometer, nitrogen ingress pipe are housed, feed nitrogen in the 250ml four-hole boiling flask reactor of reflux exchanger (on adorn drying tube), water vapour is driven away in heating, removes thermal source after reaching 100 ℃.When treating that temperature drops to about 70 ℃, add 3.65g (0.15mol) magnesium powder, 2g2-chlorobutane, 30mL ether and an iodine, slowly stir, make that material is stable in the reactor refluxed 10～20 minutes, controlled temperature is about 34 ℃.In the reactor liquid become brown, treat that reddish-brown is taken off after, beginning slowly drips Sec-Butyl Chloride solution, Sec-Butyl Chloride solution is mixed by 15g2-chlorobutane and 110mL ether; Control reaction temperature after dropwising, continued stirring reaction 3 hours at 33 ℃～35 ℃, added the hexane solution that 60mL contains the 2.5mol/L n-Butyl Lithium then in reactor fast, reduced stirring velocity, and control reaction temperature is 0 ℃～5 ℃.React the filtering separation that finishes, filtrate is analyzed Mg content with EDTA (complexometry), and calculating product yield is 85%.
Embodiment 2:
To agitator, dropping funnel, thermometer, nitrogen ingress pipe are housed, feed nitrogen in the 250ml four-hole boiling flask reactor of reflux exchanger (on adorn drying tube), water vapour is driven away in heating, removes thermal source after reaching 100 ℃.When treating that temperature drops to about 70 ℃, add 3.65g (0.15mol) magnesium powder, 2g2-chlorobutane, 30mL normal hexane and an iodine, slowly stir, controlled temperature is about 65 ℃.Liquid becomes rose in the bottle, treats that rose takes off, and slowly drips Sec-Butyl Chloride solution, and Sec-Butyl Chloride solution is mixed by 15g2-chlorobutane and 110mL normal hexane; Temperature of reaction is controlled at 60 ℃～68 ℃, continues stirring reaction 3 hours, adds the hexane solution that 60mL contains the 2.5mol/L n-Butyl Lithium then in reactor fast, reduces stirring velocity, and control reaction temperature is 0 ℃～5 ℃.React the filtering separation that finishes, filtrate is analyzed Mg content with EDTA, and calculating product yield is 75%.
Embodiment 3:
To agitator, dropping funnel, thermometer, nitrogen ingress pipe are housed, feed nitrogen in the 250ml four-hole boiling flask reactor of reflux exchanger (on adorn drying tube), water vapour is driven away in heating, removes thermal source after reaching 100 ℃.When treating that temperature drops to about 70 ℃, add 4.4g (0.18mol) magnesium powder, 3g2-chlorobutane, 100mL ether and iodine, slowly stir, controlled temperature is about 33 ℃.Liquid becomes reddish-brown in the bottle, treats that reddish-brown takes off, and slowly drips Sec-Butyl Chloride solution, and Sec-Butyl Chloride solution is mixed by 14g2-chlorobutane and 160mL ether.Temperature of reaction is controlled at 33 ℃～35 ℃, continues stirring reaction 3 hours, adds the hexane solution that 60mL contains the 2.5mol/L n-Butyl Lithium then in reactor fast, reduces stirring velocity, and control reaction temperature is 0 ℃～5 ℃.React the filtering separation that finishes, filtrate is analyzed Mg content with EDTA, and calculating product yield is 76%.
Embodiment 4:
To agitator, dropping funnel, thermometer, nitrogen ingress pipe are housed, feed nitrogen in the 250ml four-hole boiling flask reactor of reflux exchanger (on adorn drying tube), water vapour is driven away in heating, removes thermal source after reaching 100 ℃.When treating that temperature drops to about 70 ℃, add 4.9g (0.2mol) magnesium powder, 2g2-chlorobutane, 30mL normal hexane and an iodine, slowly stir, controlled temperature is about 65 ℃.Liquid becomes rose in the bottle, treats that rose takes off, and slowly drips Sec-Butyl Chloride solution, and Sec-Butyl Chloride solution is mixed by 15g2-chlorobutane and 110mL normal hexane; Temperature of reaction is controlled at 60 ℃～68 ℃, continues stirring reaction 3 hours, adds the hexane solution that 60mL contains the 2.5mol/L n-Butyl Lithium then in reactor fast, reduces stirring velocity, and control reaction temperature is 0 ℃～5 ℃.React the filtering separation that finishes, filtrate is analyzed Mg content with EDTA, and calculating product yield is 76.6%.
Claims (7)
1, a kind of preparation method of dibutylmagnesium is characterized in that: with Sec-Butyl Chloride, magnesium powder, n-Butyl Lithium is raw material, synthetic dibutylmagnesium under anhydrous, anaerobic solvent condition, and its reaction process comprises: at N
2Protection mixes magnesium powder, initiator down, places the reactor heating, stirs, and slowly add a small amount of Sec-Butyl Chloride solution, after the initiation reaction, under the insulation situation, Sec-Butyl Chloride solution is slowly added reactor, and reaction generates Grignard reagent CH
3CH
2CH (CH
3) MgCl; Cool, add the n-Butyl Lithium hexane solution fast, after the insulation reaction, fractionation by distillation goes out solvent, and cold filtration prepares dibutylmagnesium; Each proportion of raw materials is in the preparation process: magnesium powder: Sec-Butyl Chloride: the mol ratio of n-Butyl Lithium is 1.0～1.2: 1: 1.
2, by the preparation method of the described dibutylmagnesium of claim 1, it is characterized in that described initiator is I
2, Br
2, methyl iodide, monobromethane or Grignard reagent; The add-on of described initiator is 0.1～0.5 ‰ of Sec-Butyl Chloride institute consumption by weight.
3, by the preparation method of the described dibutylmagnesium of claim 1, it is characterized in that described reactor is to have in the reactor of stirring, reflux exchanger, nitrogen ingress pipe, dropping funnel, reaction process feeds nitrogen.
4, by the preparation method of the described dibutylmagnesium of claim 1, it is characterized in that after reaction causes, Sec-Butyl Chloride solution slowly being dropped in the reactor, temperature of reaction is controlled at 30 ℃～100 ℃; After dropwising, continue to stir insulation reaction 1.5～3 hours.
5,, it is characterized in that after generating Grignard reagent, cooling by the preparation method of the described dibutylmagnesium of claim 1, under 0 ℃～60 ℃ temperature, add the n-Butyl Lithium hexane solution fast, insulation reaction 1～2 hour, holding temperature are controlled at 30 ℃～120 ℃.
6, press the preparation method of the described dibutylmagnesium of claim 1, it is characterized in that described Sec-Butyl Chloride solution is formulated by Sec-Butyl Chloride and solvent, strength of solution is 0.6～1.05mol/L, and described solvent is an ether, or is in tetrahydrofuran (THF), benzene, toluene, the normal hexane any one.
7, by the preparation method of the described dibutylmagnesium of claim 1, it is characterized in that described n-Butyl Lithium hexane solution is formulated by n-Butyl Lithium and solvent normal hexane, the volumetric molar concentration of solution is 2.5mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101968974A CN101362772A (en) | 2008-09-09 | 2008-09-09 | The preparation method of dibutylmagnesium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101968974A CN101362772A (en) | 2008-09-09 | 2008-09-09 | The preparation method of dibutylmagnesium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101362772A true CN101362772A (en) | 2009-02-11 |
Family
ID=40389398
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|---|---|---|---|
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Cited By (1)
| 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 |
-
2008
- 2008-09-09 CN CNA2008101968974A patent/CN101362772A/en active Pending
Cited By (1)
| 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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