CN1217948C - Production method of alkyl lithium - Google Patents
Production method of alkyl lithium Download PDFInfo
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- CN1217948C CN1217948C CN 03118209 CN03118209A CN1217948C CN 1217948 C CN1217948 C CN 1217948C CN 03118209 CN03118209 CN 03118209 CN 03118209 A CN03118209 A CN 03118209A CN 1217948 C CN1217948 C CN 1217948C
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- lithium
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- sand
- slurry tank
- butyl chloride
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 98
- -1 alkyl lithium Chemical compound 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 83
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000004576 sand Substances 0.000 claims abstract description 23
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 23
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000002893 slag Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 239000007790 solid phase Substances 0.000 claims abstract description 5
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 20
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 13
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- 238000004062 sedimentation Methods 0.000 claims description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000009849 deactivation Effects 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 229930195733 hydrocarbon Natural products 0.000 abstract description 3
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000004215 Carbon black (E152) Substances 0.000 abstract 2
- 238000003825 pressing Methods 0.000 abstract 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 239000007788 liquid Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 229910052786 argon Inorganic materials 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000002826 coolant Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methylcyclopentane Chemical compound CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010539 anionic addition polymerization reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000005826 halohydrocarbons Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention provides a production method of alkyl lithium, which comprises the steps of dispersing a metal lithium ingot into lithium sand with the particle size of 20-400 mu m under a closed condition by using white oil with the water value of 100-300 mg/kg as a dispersing agent; transferring the lithium sand to a synthesis kettle, adding a certain amount of hydrocarbon solvent, adjusting the volume of the hydrocarbon solvent, calculating the addition amount of chlorohydrocarbon according to the 5-7% excess of lithium to chlorohydrocarbon, adding chlorohydrocarbon in a dropwise adding mode, controlling the reaction temperature to be 70-85 ℃, and controlling the reaction temperature to ensure that chlorohydrocarbon is completely converted; pressing the materials into a settling tank after the synthesis reaction is finished, standing, extracting the alkyllithium solution containing a small amount of solid-phase impurities at the upper layer after lithium slag in the solution is fully settled, and performing filter pressing through a filter or a filter to obtain the alkyllithium solution. The method has high reaction temperature and improves the production capacity in unit time; the raw material proportion is low, the consumption and the product cost are reduced, and the alkyllithium solution with the mass percentage as high as 25 percent can be directly produced.
Description
Technical field
The present invention relates to a kind of production method of lithium alkylide.
Technical background
Mainly as the initiator of anionoid polymerization, its demand increases very fast lithium alkylide at present.In the prior art, report synthetic about lithium alkylide and preparation is many, as the United States Patent (USP) over past ten years U.S.P.5 is just arranged, 332,533 (1994), 5,340,507 (1994), 5,567,474 (1996), 5,776,396 (1998) or the like.The synthetic employing chloroparaffin of lithium alkylide and the route that metallic lithium sand reacts in varsol.Owing to be the restriction that thermopositive reaction adds side reaction, temperature of reaction generally is controlled at 35 ℃～55 ℃, reaction time is long, production capacity is low, in order to prevent that residual chloroparaffin is to the influence of polymerization process in the product, usually the excessive 12%-25% of lithium that price is higher to guarantee the completely consumed of another reactant chloroparaffin, causes whole process very uneconomical thus.
Summary of the invention
Lithium alkylide is as anionic polymerization initiator, and its development prospect is boundless, and commodity amount also improves year by year.The industrial production of lithium alkylide need adopt low cost, high-level efficiency and very safe technology, how to make the maximum more cheap product of device output of certain scale seem extremely important.In addition, the common and polymkeric substance factory close together of the technical scale device of lithium alkylide is so that provide the high reactivity initiator for it.Owing to can directly send to pipeline, there is not transportation problem, lithium alkylide concentration can meet the demands about 10% in the case, and easy to implement in actual production.But, will prepare the lithium alkylide of high density, so that whole process is more economical if consider to store and transportation problem.Usual method is to adopt decompression or routine to distill the solvent of removing in the lower concentration alkyl lithium solution, but this method needs heating, and the decomposition temperature of lithium alkylide is generally lower, and side reaction takes place easily, thereby influences the lithium alkylide activity.
The object of the present invention is to provide a kind of simple, safe and economic production method, make that the lithium alkylide productive rate improves, cost descends, and can directly obtain the alkyl lithium solution of higher concentration, make its storage and during as the transportation of goods expense more cheap.
To achieve these goals, the present invention has adopted following technical scheme: be that the white oil of 100mg/kg～300mg/kg is made the lithium sand that dispersion agent is dispersed into the metallic lithium ingot 20 μ m～400 μ m with water number in confined conditions 1); 2) lithium sand is transferred to synthesis reactor, with varsol (varsol can be industrial hexanaphthene or industrial hexane or raffinate oil or mixture between them) that the lithium sand washing that the Scattered Kettle inwall adheres to is clean, continue to add solvent to adjust the total solvent amount at prescribed value toward synthesis reactor, press lithium and calculate the n-butyl chloride add-on than the excessive 5%-7% of n-butyl chloride, adopt the dropping mode to add n-butyl chloride, control reaction temperature is at 70 ℃～85 ℃, the reinforced time 1.5h～6h of control, total reaction time is 4h～8h, and n-butyl chloride is transformed fully; 3) after building-up reactions is finished material is pressed into slurry tank, leaves standstill, treat lithium slag (LiCl, Li in the solution
3N, unreacted metal lithium etc.) fully extract the alkyl lithium solution that the upper strata contains a small amount of solid phase impurity after the sedimentation, through filter or filter press filtration, obtain alkyl lithium solution.
The process flow diagram of specific implementation process of the present invention is seen accompanying drawing 1.Earlier with Scattered Kettle (1) argon replaces 1 time～3 times, add the white oil that metallic lithium ingot and water number are 100mg/kg～300mg/kg again, with logical last 200 ℃～250 ℃ heating agent of Scattered Kettle chuck, after confirming the complete fusion of metallic lithium, start stirring (rotating speed is 3000rpm) it is separated into very thin drop.Behind 10min～30min heating agent is switched to refrigerant, when material in the still drops to 150 ℃～180 ℃ (below the metallic lithium fusing point), stop to stir.This moment, metallic lithium became the dispersion that particle diameter is 20 μ m～400 μ m, continues logical refrigerant it is reduced to below 60 ℃.
Use argon replaces 1 time～3 times in the synthesis reactor (2), lithium sand in the Scattered Kettle is put into, with varsol (varsol can be industrial hexanaphthene or industrial hexane or raffinate oil or mixture between them) that the lithium sand washing that the Scattered Kettle inwall adheres to is clean, continue to add solvent to adjust the total solvent amount at prescribed value toward synthesis reactor.Press lithium and calculate the n-butyl chloride add-on than the excessive 5%-7% of n-butyl chloride.70 ℃～85 ℃ of control reaction temperature adopt the dropping mode to add n-butyl chloride, reinforced time 1.5h～6h, and total reaction time is 4h～8h.Synthesis reactor is a closed system during reaction, allows OMPa～0.15MPa pressure (gauge pressure).Exothermic heat of reaction is taken away with water coolant.The reaction and the side reaction of metallic lithium and halohydrocarbon are as follows in the synthesis reactor.
Material behind synthetic the finishing is pressed into slurry tank (3), leave standstill 4h～8h after, reaction product LiCl, Li
3N, unreacted metal lithium and alkyl lithium solution natural layering, extract by bottom insert canal that the alkyl lithium solution contain a small amount of solid phase impurity is transparent through the colourless or little Huang of filtrate that filter or filter (4) press filtration obtain, no suspended substance, quality percentage composition be up to 25% alkyl lithium solution, product concentration can be easily by adjusting quantity of solvent and the change processing condition realize.
For improving yield, can be by adding solvent soaking in a small amount of alkyl lithium solution remaining bottom slurry tank, sedimentation, press filtration are reclaimed.
By product LiCl, unreacted metal lithium that slurry tank bottom is remaining and the Li that generates when filtering
3N (merging is called the lithium slag) delivers to hydrolysis kettle (5), adds water and the lithium pulp water is separated lose activity, be converted into LiCl and LiOH.
The synthetic of lithium alkylide is strong exothermal reaction, is example with the n-Butyl Lithium, sees reaction formula:
ΔH
f(KJ.mol
-1)0 -188 -134 -402
ΔH
r＝-348(KJ.mol
-1)
Therefore to the selection and the design of reactor, at first should be taken into account the problem of heat transfer.In addition, the proportion of metallic lithium is 0.534 (20 ℃), and is more much smaller with the proportion of the n-butyl chloride of reaction usefulness than reaction solvent, so the whipped-up structure of reactor must be able to guarantee that lithium disperses thing and n-butyl chloride fully to act on.
Compared with prior art, the present invention has following tangible advantage:
1, adopting water number is the dispersion agent of the white oil of 100mg/kg～300mg/kg as preparation lithium sand, does not need to add in addition other dispersion agents and can reach effect preferably, and the lithium sand that obtains is used for lithium alkylide reacting balance when synthetic, yield height.Because of lithium sand surface coverage with LiOH, not gelling, do not tie plate.
2, higher temperature of reaction has improved unit time throughput.
Because thermal discharge was very big when lithium alkylide was synthetic, control lower temperature difficulty relatively, need realize by prolonging the reaction times.After temperature improved, building-up process was more easy to control, and the reaction times shortens greatly, and unit time throughput is original 3 times～4 times.High temperature is synthetic can also to make the n-butyl chloride reaction more complete, can improve the yield of product.
3, optimum material proportion has reduced consumption and product cost.
The excessive value that the present invention controls lithium is 5%～7%, is 1/3～1/2 of prior art; The consumption of lithium and the cost of product have been effectively reduced.
4, the present invention can direct production obtain the quality percentage composition up to 25% alkyl lithium solution.
Description of drawings
Fig. 1 is a process flow diagram; In Fig. 1: 1-Scattered Kettle, 2-synthesis reactor, 3-slurry tank, 4-strainer or filter, 5-hydrolysis kettle.
Embodiment
Embodiment 1: the Scattered Kettle that with volume is 250L is with argon replaces 2 times, and adding water number again and be the 26# industrial white oil 70L of 132ppm and 14.10kg, to contain the sodium amount be 1.5 (wt) % metallic lithium ingot.Again chuck is with heat-conducting oil heating 1～2h after replacing 2 times with argon gas, and the high-shear that starts rotating speed and be 2960rpm after the whole fusions of metallic lithium in the still is stirred.Behind the 10min deep fat is switched to cold oil rapidly, when temperature in the kettle is reduced to 170 ℃, stop to stir, continue cooling and obtain the lithium sand of particle diameter between 15～400 μ m.The synthesis reactor (band multilayer mechanical stirring) that with volume is 1500L is put into lithium sand, white oil in the Scattered Kettle wherein then with argon replaces 2 times, also puts into synthesis reactor after washing Scattered Kettle with the 200L hexanaphthene.Repeat above step twice (amount of each lithium is slightly different) 41.83kg lithium sand is added synthesis reactor.Start and use volume pump in still, to drip 294.2L n-butyl chloride (lithium is than theoretical value excessive about 6%), the chuck cooling water temperature after synthesis reactor stirs.Reinforced finishing behind the 2h cut off water coolant and continues Synthetic 2 h, and controlling whole process reaction temperature is 75～85 ℃.Material behind synthetic the finishing is pressed into slurry tank, extract the past strainer of alkyl lithium solution pressure that the upper strata contains a small amount of solid phase impurity with nitrogen from bottom insert canal after leaving standstill 8h, obtaining 780L concentration is the pale yellow transparent butyl lithium solution of 2.63M, and active C-Li content is 98.2%, residual BuCl content is 0.02%, Cl
-Content is 57ppm.In slurry tank, add the 1200L hexanaphthene, draw up portion's clear liquid behind the sedimentation 4h and filter the butyl lithium solution that obtains 0.41M concentration.In slurry tank, add the 600L hexanaphthene again, draw up portion's clear liquid behind the sedimentation 6h and filter the butyl lithium solution that obtains 0.13M concentration.It is 93.0% that stoste and twice clear liquid merge with the chlorobutane rate of collecting.The lithium slag enters hydrolysis kettle posthydrolysis deactivation in the slurry tank.
Embodiment 2: the Scattered Kettle that with volume is 250L is with argon replaces 2 times, and adding water number again and be the 26# industrial white oil 70L of 177ppm and 14.31kg, to contain the sodium amount be 1.5 (wt) % metallic lithium ingot.Prepare lithium sand with the method identical with executing example 1.The synthesis reactor (band multilayer mechanical stirring) that with volume is 1500L is with argon replaces 2 times, then lithium sand, white oil in the Scattered Kettle are put into wherein, (quality group becomes hexanaphthene 81.9% with the 200L varsol, hexane 14.8%, methylcyclopentane 2.3%, all the other hydro carbons 1.0%) also put into synthesis reactor behind the washing Scattered Kettle.Repeat above step twice (amount of each lithium is slightly different) 42.50kg lithium sand is added synthesis reactor.Start and use volume pump in still, to drip 302.1L n-butyl chloride (lithium is than theoretical value excessive about 5%), the chuck cooling water temperature after synthesis reactor stirs.Finish 2.2h the back is reinforced, cut off water coolant and continue Synthetic 2 h, controlling whole process reaction temperature is 70～85 ℃.It is the pale yellow transparent butyl lithium solution of 2.68M that material behind synthetic the finishing uses sedimentation, the filter method identical with executing example 1 to obtain 790L concentration, and active C-Li content is 98.4%, and residual BuCl content is 0.02%, Cl
-Content is 39ppm.With 1200L, 600L hexanaphthene slurry tank is soaked, takes out clear liquid twice successively, it is 92.7% that stoste and twice clear liquid merge with the chlorobutane rate of collecting.The lithium slag enters hydrolysis kettle posthydrolysis deactivation in the slurry tank.
Embodiment 3: prepare lithium sand 42.17kg and put into synthesis reactor by executing example 1 method with the 26# industrial white oil of water number 179ppm and the metallic lithium ingot of sodium content 1.5 (wt) %, altogether with 750L hexanaphthene washing Scattered Kettle.In synthesis reactor, drip 294.1L n-butyl chloride (lithium is than theoretical value excessive about 7%) by executing example 1 step, it is the pale yellow transparent butyl lithium solution of 2.31M that the synthetic after-filtration that finishes obtains 930L concentration, active C-Li content is 98.9%, and residual BuCl content is 0.01%, Cl
-Content is 37ppm.It is 92.7% with the chlorobutane rate of collecting that the clear liquid merging is taken out in twice sedimentation.The lithium slag enters hydrolysis kettle posthydrolysis deactivation in the slurry tank.
The comparative example 1: the hexanaphthene of lithium sand that 14.33kg is prepared and 70L dispersion medium white oil, 600L washing Scattered Kettle is put into synthesis reactor (concrete steps are with executing example 1).In still, drip 93.8L n-butyl chloride (lithium is than theoretical value excessive about 14%), control reaction temperature is 35-55 ℃, and all the other are by executing example 1 reaction, filtering that to obtain 430L concentration be the pale yellow transparent butyl lithium solution of 1.10M, and active C-Li content is 98.3%, residual BuCl content is 1.09%, Cl
-Content is 275ppm.Add the 800L hexanaphthene in slurry tank, draw up portion's clear liquid behind the sedimentation 4h and filter the butyl lithium solution that obtains 0.26M concentration, both merge with the chlorobutane rate of collecting is 76.6%.The lithium slag enters hydrolysis kettle posthydrolysis deactivation in the slurry tank.
The comparative example 2: the industrial hexanaphthene (forming with executing example 2) of lithium sand that 14.07kg is prepared and 70L dispersion medium white oil, 600L washing Scattered Kettle is put into synthesis reactor (concrete steps are with executing example 1).In still, drip 88.2L n-butyl chloride (lithium is than theoretical value excessive about 19%), control reaction temperature is 35-55 ℃, and all the other are by executing example 1 reaction, filtering that to obtain 430L concentration be the pale yellow transparent butyl lithium solution of 1.08M, and active C-Li content is 98.7%, residual BuCl content is 0.89%, Cl
-Content is 313ppm.Add the 800L hexanaphthene in the slurry tank, taking out after the clear liquid that both merge with the chlorobutane rate of collecting is 79.8%.The lithium slag enters hydrolysis kettle posthydrolysis deactivation in the slurry tank.
Claims (5)
1, a kind of production method of lithium alkylide is characterized in that 1) be that the white oil of 100mg/kg～300mg/kg is made the lithium sand that dispersion agent is dispersed into the metallic lithium ingot 20 μ m～400 μ m with water number in confined conditions; 2) lithium sand is transferred to synthesis reactor, with varsol that the lithium sand washing that the Scattered Kettle inwall adheres to is clean, continue to add solvent to adjust the total solvent amount at prescribed value toward synthesis reactor, press lithium and calculate the n-butyl chloride add-on than the excessive 5%-7% of n-butyl chloride, adopt the dropping mode to add n-butyl chloride, control reaction temperature is controlled reinforced time 1.5h～6h at 70 ℃～85 ℃, total reaction time is 4h～8h, and n-butyl chloride is transformed fully; 3) after building-up reactions is finished material is pressed into slurry tank, leaves standstill, treat to extract the alkyl lithium solution that the upper strata contains a small amount of solid phase impurity after the abundant sedimentation of lithium slag in the solution,, obtain alkyl lithium solution through filter or filter press filtration.
2, method according to claim 1 is characterized in that varsol is industrial hexanaphthene or industrial hexane or raffinates oil or the mixture between them.
3, method according to claim 1 and 2 is characterized in that the remaining a small amount of alkyl lithium solution in slurry tank bottom is passed through to add solvent soaking, and sedimentation, press filtration are reclaimed.
4, method according to claim 1 and 2 is characterized in that the remaining lithium slag in slurry tank bottom delivers to the hydrolysis kettle deactivation that is hydrolyzed, and makes it to be converted into LiCl and LiOH.
5, method according to claim 3 is characterized in that the remaining lithium slag in slurry tank bottom delivers to the hydrolysis kettle deactivation that is hydrolyzed, and makes it to be converted into LiCl and LiOH.
Priority Applications (1)
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|---|---|---|---|
| CN 03118209 CN1217948C (en) | 2003-03-21 | 2003-03-21 | Production method of alkyl lithium |
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|---|---|---|---|
| CN 03118209 CN1217948C (en) | 2003-03-21 | 2003-03-21 | Production method of alkyl lithium |
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| CN1217948C true CN1217948C (en) | 2005-09-07 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102952955B (en) * | 2012-11-11 | 2014-04-30 | 新疆科源化工有限公司 | Method for cleaning lithium cleaner |
| CN103435634B (en) * | 2013-07-30 | 2015-09-30 | 上虞华伦化工有限公司 | A kind of preparation method of hexyllithium |
| CN106582854B (en) * | 2015-10-19 | 2019-05-14 | 中国石油化工股份有限公司 | Allyl acetate catalyst and its application |
| CN106380476A (en) * | 2016-08-29 | 2017-02-08 | 北京百灵威科技有限公司 | Filtration method for removing solid impurities in organometallic reagent or solution |
| CN106928256A (en) * | 2017-05-15 | 2017-07-07 | 江苏维祥生物科技有限公司 | A kind of method for preparing s-butyl lithium |
| RU2691649C1 (en) * | 2019-02-01 | 2019-06-17 | Владимир Стефанович Глуховской | Method of producing alkyl lithium |
| CN113735670A (en) * | 2021-08-28 | 2021-12-03 | 江西赣锋锂业股份有限公司 | Method for industrially producing sec-butyl lithium |
| CN116284060B (en) * | 2023-05-22 | 2023-08-01 | 研峰科技(北京)有限公司 | Safe production process of organic lithium reagent butyl lithium |
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Owner name: CHINA PETROCHEMICAL CORPORATION; BALING PETROCHEM Free format text: FORMER OWNER: BALING PETROCHEMICAL CO., LTD., SINOPEC Effective date: 20070622 |
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Effective date of registration: 20070622 Address after: 100029 No. 6, Xin Xin Street East, Beijing, Chaoyang District Co-patentee after: China Petrochemical Group Baling Petroleum Co.,Ltd. Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Address before: 414014 Hunan Province, Yueyang City Patentee before: China Petrochemical Group Baling Petroleum Co.,Ltd. |
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Granted publication date: 20050907 |