CN101100473A - Method for purifying n-butyl lithium - Google Patents
Method for purifying n-butyl lithium Download PDFInfo
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- CN101100473A CN101100473A CNA2006100523137A CN200610052313A CN101100473A CN 101100473 A CN101100473 A CN 101100473A CN A2006100523137 A CNA2006100523137 A CN A2006100523137A CN 200610052313 A CN200610052313 A CN 200610052313A CN 101100473 A CN101100473 A CN 101100473A
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- butyl lithium
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Abstract
A method for purifying n-butyl lithium is carried out by delivering n-butyl lithium solution containing impurities into shaft settling tank, settling naturally, entering filtrate into centrifuge, enclosing while filtering, passing the obtained filtrate into micro-porous filter, inducing inert gas into micro-porous filter, filtering impurities with particle size 1-4 micron to obtain light-yellow transparent liquor. It's efficient, has less consumption and higher purity.
Description
Technical field
The present invention relates to chemical field, specifically a kind of purification process of n-Butyl Lithium.
Background technology
N-Butyl Lithium, molecular formula C
4H
9Li, molecular weight is 64.05, is a kind of anionic polymerization initiator that is widely used in industries such as medication chemistry, liquid crystal electron, rubber, scientific research and foodstuff additive.Its world market major part is by some large-scale manufacturer monopolization controls of the U.S..Domestic except that Ba Ling petrochemical industry and Yueyang general petrochemicals factory for its rubber chemicals inside forms a complete production network, almost do not have other manufacturer, say nothing of supplier's grade n-Butyl Lithium.
Because domestic manufacturer is supporting personal, and the product foreign matter content is required not really strictness, so they only make simple separating and filtering to the n-Butyl Lithium product.Petrochemical technology, 1999,6 (2): 91-94, mention " earlier being that the butyllithium reaction solution of 5%-10% is sent into the natural subsidence jar and carried out gravity settling; the solid residue of 80%-90% is settled down, and natural subsidence jar top is to contain the clear liquid of particle diameter less than 15 μ m solid particulates in " discussion of butyllithium filtration process technology " with solid content.Under 0.1Mpa-0.3Mpa pressure, this part clear liquid is pressed into strainer filters, the small solid particulate of particle diameter between 4-15 μ m effectively to be tackled, qualified filtrate is sent to the butyllithium storage tank, filter residue then is pressed into the residue jar by rinse solvent ".What above-mentioned filter method adopted is the filter type of drum type brake, filtration is carried out having under the water aerobic situation, because butyllithium is a heat-sensitive substance, can react with water, oxygen, butyllithium is incurred loss, and the product purity that obtains can not satisfy the commercialization requirement, especially can not satisfy the needs of medication chemistry, liquid crystal electron and scientific research.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective that above-mentioned prior art exists, a kind of three step of anhydrous and oxygen-free filtration method of n-Butyl Lithium is provided, can effectively remove the impurity alkali in the n-Butyl Lithium, improve product purity, make product satisfy the commercialization requirement, especially satisfy the needs of medication chemistry, liquid crystal electron and scientific research.
The present invention adopts following technical scheme: the purification process of n-Butyl Lithium, its step is as follows: a) impure n-butyllithium solution is sent into and carried out vertical natural subsidence in the vertical subsider, filter out in the solution about about 70% lithium chloride impurity, adopt vertical sedimentation to filter for a long time, treat that filter residue runs up to and clean again after a certain amount of, increase work efficiency; B) filtrate of a step gained enters and airtightly in the whizzer gets rid of filter, filters out about 28% lithium chloride impurity; C) filtrate of b step gained is sent into millipore filter and is filtered, and feeds rare gas element simultaneously in millipore filter, is particle diameter that 1～4 micron impurity filters, light yellow transparent liquid; Above-mentioned three step purification steps all carry out the anhydrous and oxygen-free filter operation in sealed vessel.The present invention sets about (, grain big as viscosity is thin etc.) from the physicochemical property of impurity alkali (being lithium chloride), in conjunction with the n-Butyl Lithium own characteristic, by theoretic discussion and test comparison repeatedly, determine to adopt three step of above-mentioned anhydrous and oxygen-free filtration method to remove the impurity lithium chloride at last.
As further technical scheme of the present invention, the filtrate elder generation of b step gained in middle turn trough, sends into millipore filter by pipe-line transportation then.Solution work output in controlling according to the filtration yield of millipore filter in the turn trough is avoided the strainer overload operation.
As further technical scheme of the present invention, described vertical subsider is equipped with vertical web plate and anti-clogging plug recoiling device, adopts vertical web plate, filter opening on it is difficult for being stopped up by impurity, the filtration efficiency height, and do not need frequent cleaning, the used time is 0.5～3 hour during natural subsidence.
As further technical scheme of the present invention, the filtrate of b step gained is got rid of filter under non-negative pressure, prevent in the air admission whizzer that the time is 5～40 minutes.
As further technical scheme of the present invention, consider from n-Butyl Lithium filtration process and economy angle, the pressure≤0.06Mpa during millipore filtration, the excessive filtration velocity on the contrary of pressure is slow, and filtration time is 1～4 hour.
The present invention removes the impurity lithium chloride by three step filtration methods under anhydrous and oxygen-free, have following beneficial effect: filter under anhydrous, anaerobic, avoided the loss of n-Butyl Lithium; Adopt vertical sedimentation to filter for a long time, treat that filter residue runs up to clean again after a certain amount of, improved working efficiency; The purity height of products obtained therefrom has satisfied the commercialization requirement, has especially satisfied the needs of medication chemistry, liquid crystal electron and scientific research.
Below by specific embodiment the present invention is further specified, but embodiment is not a limitation of the present invention.
Embodiment
Embodiment 1: impure n-butyllithium solution is put into vertical subsider by pipeline, after about 1 hour of the natural subsidence, filtrate enters by pipeline and gets rid of filter 15 minutes in the whizzer, filtrate again by pipe-line transportation to middle turn trough, enter millipore filter, in millipore filter, feed argon gas (pressure-controlling in the strainer is at 0.05Mpa), filtered 2 hours, the impurity of particle diameter at 1～4 micron is filtered, get light yellow transparent liquid.After testing, the major impurity content of products obtained therefrom is 0.86%.
Embodiment 2: impure n-butyllithium solution is put into vertical subsider by pipeline, after about 2 hours of the natural subsidence, filtrate enters by pipeline and gets rid of filter 15 minutes in the whizzer, filtrate again by pipe-line transportation to middle turn trough, enter millipore filter, in millipore filter, feed argon gas (pressure-controlling in the strainer is at 0.06Mpa), filtered 2 hours, the impurity of particle diameter at 1～4 micron is filtered, get light yellow transparent liquid.After testing, the major impurity content of products obtained therefrom is 0.67%.
Embodiment 3: impure n-butyllithium solution is put into vertical subsider by pipeline, after about 2 hours of the natural subsidence, filtrate enters by pipeline and gets rid of filter 10 minutes in the whizzer, filtrate again by pipe-line transportation to middle turn trough, enter millipore filter, in millipore filter, feed argon gas (pressure-controlling in the strainer is at 0.06Mpa), filtered 2 hours, the impurity of particle diameter at 1～4 micron is filtered, get light yellow transparent liquid.After testing, products obtained therefrom major impurity content is 0.69%.
Embodiment 4: impure n-butyllithium solution is put into vertical subsider by pipeline, after about 2 hours of the natural subsidence, filtrate enters by pipeline and gets rid of filter 15 minutes in the whizzer, filtrate again by pipe-line transportation to middle turn trough, enter millipore filter, in millipore filter, feed argon gas (pressure-controlling in the strainer is at 0.05Mpa), filtered 1.5 hours, the impurity of particle diameter at 1～4 micron is filtered, get light yellow transparent liquid.After testing, products obtained therefrom major impurity content is 0.72%.
Embodiment 5: impure n-butyllithium solution is put into vertical subsider by pipeline, after about 2 hours of the natural subsidence, filtrate enters by pipeline and gets rid of filter 15 minutes in the whizzer, filtrate again by pipe-line transportation to middle turn trough, enter millipore filter, in millipore filter, feed argon gas (pressure-controlling in the strainer is at 0.06Mpa), filter 23 hour, the impurity of particle diameter at 1～4 micron is filtered, get light yellow transparent liquid.After testing, products obtained therefrom major impurity content is 0.68%.
Embodiment 6: impure n-butyllithium solution is put into vertical subsider by pipeline, after about 2 hours of the natural subsidence, filtrate enters by pipeline and gets rid of filter 25 minutes in the whizzer, filtrate again by pipe-line transportation to middle turn trough, enter millipore filter, in millipore filter, feed argon gas (pressure-controlling in the strainer is at 0.06Mpa), filtered 2 hours, the impurity of particle diameter at 1～4 micron is filtered, get light yellow transparent liquid.After testing, products obtained therefrom major impurity content is 0.71%.
The above embodiments all are to carry out the anhydrous and oxygen-free filter operation in the container of sealing.
Claims (5)
1, the purification process of n-Butyl Lithium, its step is as follows: a) impure n-butyllithium solution is sent into and carried out vertical natural subsidence in the vertical subsider; B) filtrate of a step gained enters and airtightly in the whizzer gets rid of filter; C) filtrate of b step gained is sent into millipore filter and is filtered, and feeds rare gas element simultaneously in millipore filter, the impurity of particle diameter at 1～4 micron is filtered, light yellow transparent liquid; Above-mentioned three step purification steps all carry out under anhydrous and oxygen-free.
2, the purification process of n-Butyl Lithium according to claim 1, the filtrate that it is characterized in that b step gained earlier by pipe-line transportation in middle turn trough, send into millipore filter then.
3, the purification process of n-Butyl Lithium according to claim 1 and 2 is characterized in that described vertical subsider is equipped with vertical web plate and anti-clogging plug recoiling device, and the used time is 0.5～3 hour during natural subsidence.
4, the purification process of n-Butyl Lithium according to claim 3 is characterized in that the filtrate of b step gained is got rid of filter under non-negative pressure, and the time is 5～40 minutes.
5, the purification process of n-Butyl Lithium according to claim 4, the pressure≤0.06Mpa when it is characterized in that millipore filtration, filtration time are 1～4 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100523137A CN101100473A (en) | 2006-07-05 | 2006-07-05 | Method for purifying n-butyl lithium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100523137A CN101100473A (en) | 2006-07-05 | 2006-07-05 | Method for purifying n-butyl lithium |
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| Publication Number | Publication Date |
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| CN101100473A true CN101100473A (en) | 2008-01-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2006100523137A Pending CN101100473A (en) | 2006-07-05 | 2006-07-05 | Method for purifying n-butyl lithium |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008563A (en) * | 2016-05-23 | 2016-10-12 | 北京百灵威科技有限公司 | Method for removing solid impurities in organic metal reagent solution |
| 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 |
-
2006
- 2006-07-05 CN CNA2006100523137A patent/CN101100473A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008563A (en) * | 2016-05-23 | 2016-10-12 | 北京百灵威科技有限公司 | Method for removing solid impurities in organic metal reagent solution |
| 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 |
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