CN101100473A - Purification method of n-butyl lithium - Google Patents
Purification method of n-butyl lithium Download PDFInfo
- Publication number
- 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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- China
- Prior art keywords
- butyl lithium
- filter
- filtrate
- vertical
- filtration
- Prior art date
- Legal status (The legal status 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 status listed.)
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- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000746 purification Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title abstract description 5
- 239000000706 filtrate Substances 0.000 claims abstract description 23
- 239000012535 impurity Substances 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000011261 inert gas Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 10
- 239000007789 gas Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 6
- 229940079593 drug Drugs 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000010539 anionic addition polymerization reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a purification method of n-butyl lithium. The existing method carries out filtration under the condition of water and oxygen, so that butyl lithium is lost and the obtained product has low purity. The method comprises the following steps: a) feeding the n-butyl lithium solution containing impurities into a vertical settling tank for vertical natural settling; b) the filtrate obtained in the step a enters a centrifuge for closed filtration; c) b, feeding the filtrate obtained in the step b into a microporous filter for filtering, introducing inert gas into the microporous filter, and filtering out impurities with the particle size of 1-4 microns to obtain light yellow transparent liquid; the three purification steps are carried out under anhydrous and oxygen-free conditions. The invention avoids the loss of n-butyl lithium, has high working efficiency of filtration and high purity of the obtained product.
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 | Purification method of n-butyl lithium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100523137A CN101100473A (en) | 2006-07-05 | 2006-07-05 | Purification method of n-butyl lithium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101100473A true CN101100473A (en) | 2008-01-09 |
Family
ID=39034947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006100523137A Pending CN101100473A (en) | 2006-07-05 | 2006-07-05 | Purification method of n-butyl lithium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101100473A (en) |
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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