CN102659080A - Novel method for preparing lithium aluminum hydride - Google Patents
Novel method for preparing lithium aluminum hydride Download PDFInfo
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- CN102659080A CN102659080A CN2012101568484A CN201210156848A CN102659080A CN 102659080 A CN102659080 A CN 102659080A CN 2012101568484 A CN2012101568484 A CN 2012101568484A CN 201210156848 A CN201210156848 A CN 201210156848A CN 102659080 A CN102659080 A CN 102659080A
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Abstract
The invention relates to a novel method for preparing lithium aluminum hydride. The method comprises the following steps of: 1-, fully dissolving aluminum trichloride in anhydrous ether to prepare a diethyl ether solution of the aluminum trichloride; 2-, crushing lithium hydride particles into powder by adopting a screen mesh under the protection of nitrogen; putting the crushed lithium hydride powder into diethyl ether under the protection of the nitrogen; putting into a reaction kettle, and then evenly mixing to form a uniform lithium hydride and diethyl ether suspension for later use; 3-, mixing the diethyl ether solution of the aluminum trichloride prepared in the step (1) with the lithium hydride and diethyl ether suspension prepared in the step (2) for full reaction; and 4-, collecting clear liquid into a container after byproduct lithium chloride is deposited; performing static distillation to evaporate the diethyl ether in the clear liquid to dryness to obtain a required lithium aluminum hydride solid product. The novel method for preparing the lithium aluminum hydride is simple, safe and reliable, is low in production cost and good in product quality.
Description
Technical field
The present invention relates to a kind of metal hydride, be specifically related to a kind of preparation method of novel hydrogenated aluminium lithium.
Background technology
Lithium aluminum hydride is a kind of strong reductant that can reduce organo-functional group; Stable in dry air; Hydrolysis and cause burning in damp atmosphere, the method for most typical synthesizing hydrogenated aluminium lithium are that metallic lithium at high temperature generates lithium hydride with hydrogen reaction, then with after the lithium hydride fine grinding in anhydrous diethyl ether; In the presence of initiator, generate lithium aluminum hydride with the aluminum chloride reaction; Because it will add initiator and inflammable cause, and large-scale production is obstructed, therefore exploring the new method for preparing lithium aluminum hydride is very important problem.
Application number is 87101196; Denomination of invention discloses a kind of compound method of lithium aluminum hydride for " compound method of lithium aluminum hydride "; Its content is that metallic lithium is reacted the generation lithium hydride with hydrogen at normal temperatures and pressures in the presence of solvent and catalyzer; Lithium hydride generates lithium aluminum hydride with the aluminum chloride reaction more then, and this method exists more than the by product and the problem of potential insecurity.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of preparation method, safe and reliable, the preparation method of the novel hydrogenated aluminium lithium of good product quality.
The technical scheme that the present invention adopts is:
A kind of preparation method of novel hydrogenated aluminium lithium comprises the steps:
1), aluminum chloride fully is dissolved in the anhydrous diethyl ether, is configured to the diethyl ether solution of aluminum chloride;
2) under nitrogen protection, adopt screen cloth that the lithium hydride particle is crushed into powder, and under protection of nitrogen gas, the lithium hydride powder that crushes dropped in the middle of the ether, drop into reaction kettle after, stir, form uniform lithium hydride ether suspension liquid, continue to employ;
The diethyl ether solution and step 2 of the aluminum chloride that 3), step 1) is made) the lithium hydride ether suspension liquid that makes mixes fully reaction;
4), treat that sub product lithium chloride deposition is good after, collect clear liquid in container, carry out static state and distill, with ether evaporate to dryness wherein, obtain required lithium aluminum hydride solid phase prod.
Particularly, the preparation method of this novel hydrogenated aluminium lithium comprises the steps:
1), aluminum chloride is put into earlier in the middle of the reaction kettle, in reaction kettle, adds ether then gradually, adopt the method for measuring fixed amount, after adding a certain amount of ether, stop to feed in raw material.Open and stir, at this moment will control stirring velocity,, after stirring fully, remaining ether is continued to join in the reaction kettle, continue to employ after stirring in order to avoid cause bumping because of the dissolution process very exothermic;
2), under nitrogen protection, adopt screen cloth that the lithium hydride particle is crushed into powder, and guarantee that its powder size is evenly qualified; The lithium hydride powder that crushes is dropped in the middle of a certain amount of ether, drop into process need and under the situation of nitrogen protection, accomplish, cause danger to prevent its moisture absorption; After dropping into reaction kettle, open and stir, it is stirred; Make it form uniform lithium hydride ether suspension liquid, continue to employ.
3), in certain temperature, open under the condition of stirring, to step 2) slowly add the diethyl ether solution of the aluminum chloride that step 1) makes in the lithium hydride ether suspension liquid that makes, adding speed must be controlled well, otherwise bumping possibly take place.Simultaneously, an amount of feeding nitrogen in reaction kettle, the whole charging process need long period, after the completion to be added, continue to stir for some time, it is fully reacted.
4), after reaction accomplishes, treat that sub product lithium chloride deposition is good after, collect clear liquid in container, carry out static state and distill, with ether evaporate to dryness wherein, obtain required lithium aluminum hydride solid phase prod.
The beneficial effect that the present invention had:
Working method of the present invention is simple, and is safe and reliable, and production cost is low, and good product quality.
Embodiment
Below in conjunction with specific embodiment the present invention is described further, but does not limit protection scope of the present invention.
Embodiment 1
A kind of preparation method of novel hydrogenated aluminium lithium comprises the steps:
1), aluminum chloride is put into earlier in the middle of the reaction kettle, in reaction kettle, adds ether then gradually, adopt the method for measuring fixed amount, after adding a certain amount of ether, stop to feed in raw material.Open and stir, at this moment will control stirring velocity,, after stirring fully, remaining ether is continued to join in the reaction kettle, continue to employ after stirring in order to avoid cause bumping because of the dissolution process very exothermic;
2), under nitrogen protection, adopt screen cloth that the lithium hydride particle is crushed into powder, and guarantee that its powder size is evenly qualified; The lithium hydride powder that crushes is dropped in the middle of a certain amount of ether, drop into process need and under the situation of nitrogen protection, accomplish, cause danger to prevent its moisture absorption; After dropping into reaction kettle, open and stir, it is stirred; Make it form uniform lithium hydride ether suspension liquid, continue to employ.
3), in certain temperature, open under the condition of stirring, to step 2) slowly add the diethyl ether solution of the aluminum chloride that step 1) makes in the lithium hydride ether suspension liquid that makes, adding speed must be controlled well, otherwise bumping possibly take place.Simultaneously, an amount of feeding nitrogen in reaction kettle, the whole charging process need long period, after the completion to be added, continue to stir for some time, it is fully reacted.
4), after reaction accomplishes, treat that sub product lithium chloride deposition is good after, collect clear liquid in container, carry out static state and distill, with ether evaporate to dryness wherein, obtain required lithium aluminum hydride solid phase prod.
The above only is preferred embodiment of the present invention, is not technical scheme of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (2)
1. the preparation method of a novel hydrogenated aluminium lithium is characterized in that: comprise the steps:
1), aluminum chloride fully is dissolved in the anhydrous diethyl ether, is configured to the diethyl ether solution of aluminum chloride;
2) under nitrogen protection, adopt screen cloth that the lithium hydride particle is crushed into powder, and under protection of nitrogen gas, the lithium hydride powder that crushes dropped in the middle of the ether, drop into reaction kettle after, stir, form uniform lithium hydride ether suspension liquid, continue to employ;
The diethyl ether solution and step 2 of the aluminum chloride that 3), step 1) is made) the lithium hydride ether suspension liquid that makes mixes fully reaction;
4), treat that sub product lithium chloride deposition is good after, collect clear liquid in container, carry out static state and distill, with ether evaporate to dryness wherein, obtain required lithium aluminum hydride solid phase prod.
2. the preparation method of novel hydrogenated aluminium lithium according to claim 1 is characterized in that: comprise the steps:
1), aluminum chloride is put into earlier in the middle of the reaction kettle, in reaction kettle, adds ether then gradually, adopt the method for measuring fixed amount, after adding a certain amount of ether, stop to feed in raw material.Open and stir, at this moment will control stirring velocity,, after stirring fully, remaining ether is continued to join in the reaction kettle, continue to employ after stirring in order to avoid cause bumping because of the dissolution process very exothermic;
2), under nitrogen protection, adopt screen cloth that the lithium hydride particle is crushed into powder, and guarantee that its powder size is evenly qualified; The lithium hydride powder that crushes is dropped in the middle of a certain amount of ether, drop into process need and under the situation of nitrogen protection, accomplish, cause danger to prevent its moisture absorption; After dropping into reaction kettle, open and stir, it is stirred; Make it form uniform lithium hydride ether suspension liquid, continue to employ.
3), in certain temperature, open under the condition of stirring, to step 2) slowly add the diethyl ether solution of the aluminum chloride that step 1) makes in the lithium hydride ether suspension liquid that makes, adding speed must be controlled well, otherwise bumping possibly take place.Simultaneously, an amount of feeding nitrogen in reaction kettle, the whole charging process need long period, after the completion to be added, continue to stir for some time, it is fully reacted.
4), after reaction accomplishes, treat that sub product lithium chloride deposition is good after, collect clear liquid in container, carry out static state and distill, with ether evaporate to dryness wherein, obtain required lithium aluminum hydride solid phase prod.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012101568484A CN102659080A (en) | 2012-05-21 | 2012-05-21 | Novel method for preparing lithium aluminum hydride |
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| CN2012101568484A CN102659080A (en) | 2012-05-21 | 2012-05-21 | Novel method for preparing lithium aluminum hydride |
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| CN102659080A true CN102659080A (en) | 2012-09-12 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104759215A (en) * | 2014-12-26 | 2015-07-08 | 车荣睿 | Preparation process for lithium aluminum hydride-tetrahydrofuran solution |
| CN106966364A (en) * | 2017-04-14 | 2017-07-21 | 车荣睿 | A kind of synthesis technique of deuterate aluminium lithium |
| CN109734053A (en) * | 2019-03-26 | 2019-05-10 | 哈尔滨工业大学 | A kind of three aluminum hydride preparation methods based on recycling ether solvent |
| CN112607706A (en) * | 2020-12-04 | 2021-04-06 | 中核建中核燃料元件有限公司 | Method for reducing activity of high-activity lithium hydride powder |
| CN114162785A (en) * | 2021-12-30 | 2022-03-11 | 北京珺政慧通科技有限公司 | Coating process of alpha-aluminum trihydride |
| CN115650264A (en) * | 2022-11-28 | 2023-01-31 | 研峰科技(北京)有限公司 | Method for efficiently recovering lithium chloride from lithium aluminum hydride preparation process |
| KR102557494B1 (en) * | 2022-12-07 | 2023-07-21 | 주식회사 알링크 | Method of preparing lithium chloride |
-
2012
- 2012-05-21 CN CN2012101568484A patent/CN102659080A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104759215A (en) * | 2014-12-26 | 2015-07-08 | 车荣睿 | Preparation process for lithium aluminum hydride-tetrahydrofuran solution |
| CN106966364A (en) * | 2017-04-14 | 2017-07-21 | 车荣睿 | A kind of synthesis technique of deuterate aluminium lithium |
| CN109734053A (en) * | 2019-03-26 | 2019-05-10 | 哈尔滨工业大学 | A kind of three aluminum hydride preparation methods based on recycling ether solvent |
| CN112607706A (en) * | 2020-12-04 | 2021-04-06 | 中核建中核燃料元件有限公司 | Method for reducing activity of high-activity lithium hydride powder |
| CN114162785A (en) * | 2021-12-30 | 2022-03-11 | 北京珺政慧通科技有限公司 | Coating process of alpha-aluminum trihydride |
| CN115650264A (en) * | 2022-11-28 | 2023-01-31 | 研峰科技(北京)有限公司 | Method for efficiently recovering lithium chloride from lithium aluminum hydride preparation process |
| KR102557494B1 (en) * | 2022-12-07 | 2023-07-21 | 주식회사 알링크 | Method of preparing lithium chloride |
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Application publication date: 20120912 |