CN216296344U - Lithium amide preparation facilities - Google Patents
Lithium amide preparation facilities Download PDFInfo
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- CN216296344U CN216296344U CN202122356897.XU CN202122356897U CN216296344U CN 216296344 U CN216296344 U CN 216296344U CN 202122356897 U CN202122356897 U CN 202122356897U CN 216296344 U CN216296344 U CN 216296344U
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- preheater
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Abstract
The utility model provides a lithium amide preparation device. The lithium amide preparation device comprises a preheater and a reaction tank, wherein the preheater is used for preheating ammonia gas, the preheater is connected with the reaction tank through a valve pipeline, an inner cavity of the valve pipeline is communicated with an inner cavity of the preheater and an inner cavity of the reaction tank, a cold ammonia gas inlet pipe, a steam inlet pipe and a steam outlet pipe are arranged on the preheater, the cold ammonia gas inlet pipe is connected with a liquid ammonia storage tank, the steam inlet pipe is communicated with the inner cavity of the preheater, the steam outlet pipe is communicated with the inner cavity of the preheater and the outside, and a coil pipe communicated with the cold ammonia gas inlet pipe is arranged inside the preheater. The device for preparing the lithium amide solves the difficult problem of preparing the lithium amide by a pyrogenic process, namely the problem of difficult reaction or the defect of low main content of the prepared lithium amide, and the like.
Description
Technical Field
The utility model relates to the technical field of lithium amide, in particular to a lithium amide preparation device.
Background
Lithium amide has a molecular formula of LiNH2, is colorless needle-shaped crystal, has a melting point of 390-400 ℃, has ammonia smell, a melting point of 390 ℃, a boiling point of 430 ℃ and a temperature of 450 ℃, starts to decompose, is insoluble in kerosene and soluble in liquid ammonia, is soluble in cold water, has a relative density of 1.178 (17.5 ℃) and is strongly hydrolyzed when being heated by water, and is super-strong alkali. The lithium ion battery is mainly used for organic synthesis, pharmaceutical manufacturing and hydrogen storage materials, and is a hydrogen storage material with good prospects with lithium hydride (LiH) and lithium imido (Li 2 NH).
At present, the preparation process for preparing lithium amide at home and abroad comprises the following steps: 1. the method has the advantages that the liquid ammonia and the metal lithium are prepared by reaction, the reaction is violent, the liquid ammonia is not easy to store, and the solution leaks; 2. the method comprises the steps of introducing ammonia gas into an organic solvent to react with lithium metal to generate 'lithium bronze', synthesizing a lithium amide wet material with olefin, and finally drying to obtain the lithium amide, wherein the obtained lithium amide has low yield and main content of less than or equal to 90%, a large amount of organic solvent is used in the preparation process, and the method is not environment-friendly.
Aiming at the defects of the process, ammonia gas and lithium metal can be directly adopted to carry out melting reaction at high temperature, however, the requirement on a reaction device for preparing lithium amide by a high-temperature melting method is high, and the improper design of the device can cause the main content of the lithium amide to be low or the lithium amide does not react.
SUMMERY OF THE UTILITY MODEL
Based on the above, the utility model provides a lithium amide preparation device which solves the problems that poor reaction and non-uniform reaction are easily caused in the process of preparing lithium amide under high-temperature melting, and the lithium amide is decomposed or does not react due to over-high local temperature.
The lithium amide preparation device comprises a preheater and a reaction tank, wherein the preheater is used for preheating ammonia gas, the preheater is connected with the reaction tank through a valve pipeline, the inner cavity of the valve pipeline is communicated with the inner cavity of the preheater and the inner cavity of the reaction tank, the preheater is provided with a cold ammonia gas inlet pipe, a steam inlet pipe and a steam outlet pipe, the cold ammonia gas inlet pipe is connected with a liquid ammonia storage tank, the steam inlet pipe is communicated with the inner cavity of the preheater, the steam outlet pipe is communicated with the inner cavity of the preheater and the outside, a coil pipe communicated with the cold ammonia gas inlet pipe is arranged in the preheater, one end of the valve pipeline is connected with the coil pipe, the other end of the valve pipeline is connected with the inlet pipe in the cavity of the reaction tank, the inlet pipe is provided with an ammonia gas outlet pipe, and the reaction tank is provided with a vent pipe and a vacuum pipe connected with a vacuum pump.
Further, the cold ammonia inlet pipe is arranged at the bottom of the left side of the preheater, the steam inlet pipe is arranged at the top of the left side of the preheater, and the steam outlet pipe is arranged at the bottom of the right side of the preheater.
Furthermore, a vacuum pressure gauge is arranged on the feeding pipe.
Furthermore, the upper end face of the reaction tank is sealed through two flanges, a metal sealing gasket is arranged between the two flanges, and the two flanges are fastened through bolts.
Furthermore, the bottom of the reaction tank is provided with supporting legs, and the number of the supporting legs is at least 3.
Furthermore, the lateral part of retort is equipped with the support palm, the setting quantity of support palm is 3 at least.
Further, the ammonia outlet pipe set up quantity be 3 at least, 3 the ammonia outlet pipe is followed the axial of inlet pipe is from last to setting gradually down.
Furthermore, the ammonia outlet pipe is fixed in below the side part of the feeding pipe in a welding mode.
According to the lithium amide preparation device, the cold ammonia gas from the liquid ammonia storage tank is preheated by the preheater, and the charged ammonia gas is uniformly distributed in the reaction tank by virtue of reasonable arrangement of the opening on the side surface of the ammonia gas pipeline in the high-temperature reaction tank, so as to perform full and uniform reaction with liquid metal lithium, and meanwhile, the generated hydrogen gas is timely discharged through the gas inlet and outlet guide pipes.
The device for preparing the lithium amide has simple process and lower cost, solves the problems of decomposition caused by violent local reaction in the preparation process of the lithium amide or reaction caused by low ammonia temperature, and effectively reduces the waste problem of raw materials caused by poor reaction.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing lithium amide according to the present invention.
Description of reference numerals:
1-cold ammonia gas inlet pipe, 2-steam gas inlet pipe, 3-coil pipe, 4-valve pipeline, 5-steam gas outlet pipe, 6-preheater, 7-feed pipe, 8-ammonia gas outlet pipe, 9-metal sealing gasket, 10-reaction tank, 11-supporting leg, 12-bolt, 13-flange, 14-vent pipe, 15-vacuum pipe, 16-supporting palm, 17-vacuum pressure gauge, 18-valve, 19-argon gas exhaust pipe and 20-argon gas inlet pipe.
Detailed Description
To facilitate an understanding of the utility model, the utility model will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Referring to fig. 1, the present invention provides a lithium amide manufacturing apparatus, including a preheater 6 and a reaction tank 10, wherein an inner cavity of the preheater is communicated with an inner cavity of the reaction tank.
Be equipped with cold ammonia admission pipe 1, steam intake pipe 2 and steam outlet duct 5 on the preheater 6, cold ammonia admission pipe and liquid ammonia storage tank are connected, the steam intake pipe with preheater inner chamber intercommunication, steam outlet duct intercommunication preheater inner chamber and external, the preheater inside be equipped with the coil pipe 3 of cold ammonia admission pipe intercommunication.
Specifically, the left side bottom of preheater 6 is equipped with cold ammonia gas admission pipe 1 the left side top of preheater is equipped with steam intake pipe 2 the right side bottom of preheater is equipped with steam outlet duct 5. The ammonia storage tank of liquid ammonia releases the ammonia through opening the valve and gets into inside 6 preheaters, the ammonia is in heat in the inside coil pipe 3 of preheater, steam gets into through steam intake pipe 2 the preheater is inside right the ammonia in the coil pipe heats, then follows again 5 go out of steam outlet duct, form a passageway.
Preheater 6 with retort 10 is connected through detachably valve pipeline 4, valve pipeline 4's one end and coil pipe 3 are connected, the other end of valve pipeline and the inlet pipe 7 on the retort are connected.
And a vacuum pressure gauge 17 is arranged on the feeding pipe 7 and used for monitoring the pressure change condition in the reaction tank and adjusting the flow by controlling the pressure.
The upper end of retort 10 is equipped with vacuum tube 15 of connecting the vacuum pump, the up end of retort is sealed through two flanges 13, for guaranteeing absolute complete sealing, two install metal sealing pad 9 additional between the flange 13, metal sealing pad adopts the preparation mode of winding pad, two the flange adopts the periphery to punch to fasten with bolt 12.
Supporting legs 11 are welded on the circular periphery of the bottom of the reaction tank 10, the number of the supporting legs is 3 or more, the supporting legs are evenly distributed around the periphery, and the supporting legs are placed on the ground to play a role in supporting stability. The reaction tank 10 is placed in the electric heating furnace and supported by a support palm 16 at the upper part of the tank body, and the support palms 16 are uniformly distributed around the reaction tank and are more than 3.
The inlet pipe 7 is in retort 10's cavity, and inlet pipe 7 inserts to the distance from bottom 150mm, and the bottom mouth of pipe is sealed, adopts to weld to die, and the lateral part of inlet pipe 7 is from bottom every 10mm welding ammonia outlet duct 8, and the opening direction faces the cavity center. The ammonia outlet pipe 8 is opened every 10mm, and the number is 3 to more than, and the purpose is in order to make the even distribution of ammonia in the retort cavity, makes the reaction go on evenly.
Be equipped with breather pipe 14 on the retort, the branching of breather pipe rear end connects argon gas blast pipe 19 and argon gas intake pipe 20 respectively, is equipped with valve 18 on argon gas blast pipe 19 and the argon gas intake pipe 20 respectively, and it is gas or argon gas is given vent to anger to control argon gas with the valve during the use. In particular, the vent tube 14 is located above the flange.
The process of the device for preparing the lithium amide comprises the following steps:
step 1, putting lithium metal into a titanium plate, putting the titanium plate into a reaction tank 10 in an argon atmosphere, fastening the reaction tank through an upper flange 13, a lower flange 13, a sealing gasket 9 and a bolt 12 until the reaction tank is airtight, then hanging the reaction tank 10 into an electric heating furnace by a travelling crane to support a palm 16 stably, and setting a reaction temperature.
And 2, closing other valves, connecting the vacuum pipe with the vacuum pump, starting the vacuum pump to pump air to be within 100pa, then closing the valves on the vacuum pipe, starting the valves on the argon inlet pipe 20, filling argon for replacement for 2-3 times, and finally keeping the pressure in the cavity of the reaction tank 10 to be within 100 pa.
And 3, connecting the reaction tank 10 with a preheater 6 through a valve pipeline 4, keeping the temperature of the reaction tank 10 at a set value for 1 hour, opening a steam inlet pipe 2 and a steam outlet pipe 5, opening the valve pipeline 4, finally opening the valve pipelines of the preheater inlet pipe 1 and the liquid ammonia storage tank, and filling cold ammonia gas for preheating.
And 4, filling the preheated ammonia gas into the cavity of the reaction tank through a feed pipe 7, and uniformly distributing the ammonia gas in the cavity of the reaction tank through an outlet of an ammonia gas outlet pipe 8.
And 5, monitoring pressure change through a vacuum pressure gauge 17, wherein the pressure after inflation is not more than 0.2Mpa, opening a valve connected with an exhaust pipe 19 on an exhaust pipe 14 after ammonia gas is inflated into the reaction tank for a period of time, so that the reacted hydrogen gas can be discharged in time, wherein the discharged gas is a mixed gas of the hydrogen gas and the ammonia gas, and the mixed gas is evacuated after the ammonia gas is removed through an absorption tower.
And 6, after the gas discharge pipe is opened, maintaining the discharge balance of the ammonia gas inlet and the mixed gas, and regulating the flow rate of the flow valve through a pressure gauge 17 to keep the pressure at 0.18-0.2 MPa.
And 7, after the reaction is finished, closing steam, a switch of the electric heating furnace and all valves, after cooling, lifting out the reaction tank, placing the reaction tank on the ground by using supporting legs 11, starting a vacuum pump to pump until the negative pressure is within 100pa, then closing the vacuum pump, starting an air inlet pipe, and filling argon for replacement for 2 times.
And 8, unscrewing the bolts 12, opening the flange cover, and taking out the lithium amide to obtain the product.
The lithium amide preparation device comprises a preheater, a reaction tank, a pipeline and the like, wherein the preheater is used for preheating ammonia gas, a coil is arranged in the preheater, a heating medium is heated by steam, the steam is fed in and discharged out from the top, the ammonia gas is discharged out from the left and the right, and a valve pipeline is additionally arranged for connecting the pipeline; the reaction tank device comprises an upper flange and a lower flange, wherein the periphery of the flanges is perforated and connected by bolts, the upper flange and the lower flange are sealed by adopting metal winding pads, the tank body of the reaction tank is cylindrical, the bottom of the reaction tank is circular, the heat transfer efficiency of a reaction material and the tank bottom is increased, and the whole reaction tank is supported by adopting three or more supporting legs; the pipeline of the lithium amide preparation device comprises a feeding pipe, a vacuum pipe and a vent pipe, wherein the feeding pipe is inserted into the bottom, the bottom is sealed, the side part of the pipeline is opened at intervals, the number of the openings is three to more than three, the vacuum pipe is connected with a vacuum pump to play a role of pumping air to within 100pa so as to ensure that the whole system is almost free of air, the vent pipe is connected with two connecting pipes, one end of the vent pipe is an argon gas inlet pipe, the other end of the vent pipe is a mixed gas of hydrogen gas and ammonia gas after reaction, when the system needs gas replacement, the vent valve end is closed to fill argon gas for replacement, and when the system needs gas exhaust, the argon gas inlet valve end is closed, and the vent valve is opened to exhaust.
Further, the preheater is for preheating the ammonia, and the ammonia is outgassed from the liquid ammonia storage tank and comes, the preheater left end is cold ammonia inlet end, and the right-hand member is hot ammonia end of giving vent to anger, the preheater upper end is steam entering end, and the lower extreme is that steam condensation steam goes out the end. The ammonia gas outlet end at the right end of the preheater is connected with a valve pipeline which is connected with a feeding pipe of the reaction tank. The feed pipe of the reaction tank is connected with a vacuum pressure gauge capable of measuring negative pressure and positive pressure, and the measurement range is-0.1 MPa-0.3 MPa. The reaction tank body is cylindrical, and the bottom of the reaction tank body is circular. The bottom support of the reaction tank is a triangular support, and the side surface of the tank is also provided with a support palm which can be uniformly distributed around the tank body. The reaction tank is connected with the upper flange and the lower flange, the upper flange and the lower flange are sealed by the metal winding pad, the metal winding pad can be placed in the groove and also can be placed on the flange, holes are formed in the periphery of the upper flange and the lower flange, and the upper flange and the lower flange are fastened and connected through bolts. The retort, the metal winding pad, the bolt material can be stainless steel material also can be high temperature resistant materials such as titanium material. The pipeline is divided into a feeding pipe, a vacuum pipe and a vent pipe. The amino gas inlet pipe is inserted into the reaction tank at a distance from the bottom, the bottom opening is sealed, and the side part of the reaction tank is opened at intervals, and the number of the openings is three to more. The vacuum tube is connected with the vacuum pump, plays the effect of bleeding, and it is within 100pa to bleed to guarantee that the whole system is interior almost to have no air. The breather pipe is connected with two connecting pipes, one end of the breather pipe is an argon gas inlet pipe, and the other end of the breather pipe is a mixed gas of the reacted hydrogen and ammonia. Therefore, the pipelines are all connected by adopting stainless steel materials.
According to the lithium amide preparation device, the cold ammonia gas discharged from the liquid ammonia storage tank is preheated by the preheater, the charged ammonia gas is uniformly distributed in the reaction tank by virtue of reasonable arrangement of the opening on the side surface of the ammonia gas pipeline in the high-temperature reaction tank, the charged ammonia gas is fully and uniformly reacted with liquid metal lithium, and meanwhile, the generated hydrogen gas is timely discharged through the gas inlet and outlet guide pipe.
The above examples only express embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. An apparatus for producing lithium amide, characterized in that: comprises a preheater and a reaction tank, the preheater is used for preheating ammonia gas, the preheater is connected with the reaction tank through a valve pipeline, the inner cavity of the valve pipeline is communicated with the inner cavity of the preheater and the inner cavity of the reaction tank, the preheater is provided with a cold ammonia gas inlet pipe, a steam gas inlet pipe and a steam gas outlet pipe, the cold ammonia gas inlet pipe is connected with the liquid ammonia storage tank, the steam inlet pipe is communicated with the inner cavity of the preheater, the steam outlet pipe is communicated with the inner cavity of the preheater and the outside, a coil pipe communicated with the cold ammonia gas inlet pipe is arranged in the preheater, one end of the valve pipeline is connected with the coil pipe, the other end of the valve pipeline is connected with the feeding pipe in the cavity of the reaction tank, the ammonia gas outlet pipe is arranged on the inlet pipe, and the reaction tank is provided with a vent pipe and a vacuum pipe connected with a vacuum pump.
2. The apparatus for producing lithium amide according to claim 1, wherein: the cold ammonia inlet pipe is arranged at the bottom of the left side of the preheater, the steam inlet pipe is arranged at the top of the left side of the preheater, and the steam outlet pipe is arranged at the bottom of the right side of the preheater.
3. The apparatus for producing lithium amide according to claim 2, wherein: and a vacuum pressure gauge is arranged on the feeding pipe.
4. The apparatus for producing lithium amide according to claim 3, wherein: the upper end face of the reaction tank is sealed through two flanges, a metal sealing gasket is arranged between the two flanges, and the two flanges are fastened through bolts.
5. The apparatus for producing lithium amide according to claim 4, wherein: the bottom of the reaction tank is provided with supporting legs, and the number of the supporting legs is at least 3.
6. The apparatus for producing lithium amide according to claim 5, wherein: the lateral part of retort is equipped with the support palm, the setting quantity of support palm is 3 at least.
7. The apparatus for producing lithium amide according to claim 6, wherein: the ammonia outlet duct set up quantity be 3 at least, 3 the ammonia outlet duct is followed the axial of inlet pipe sets gradually from last to down.
8. The apparatus for producing lithium amide according to claim 7, wherein: the ammonia outlet duct adopts the welded mode to be fixed in the lateral part below of inlet pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122356897.XU CN216296344U (en) | 2021-09-28 | 2021-09-28 | Lithium amide preparation facilities |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122356897.XU CN216296344U (en) | 2021-09-28 | 2021-09-28 | Lithium amide preparation facilities |
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| CN216296344U true CN216296344U (en) | 2022-04-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115646371A (en) * | 2022-12-29 | 2023-01-31 | 研峰科技(北京)有限公司 | Lithium amide preparation facilities |
| CN116216667A (en) * | 2022-11-28 | 2023-06-06 | 江西赣锋锂业集团股份有限公司 | Industrial preparation method of lithium amide |
-
2021
- 2021-09-28 CN CN202122356897.XU patent/CN216296344U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116216667A (en) * | 2022-11-28 | 2023-06-06 | 江西赣锋锂业集团股份有限公司 | Industrial preparation method of lithium amide |
| CN115646371A (en) * | 2022-12-29 | 2023-01-31 | 研峰科技(北京)有限公司 | Lithium amide preparation facilities |
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| Date | Code | Title | Description |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 338000 Longteng Road, Xinyu Economic Development Zone, Jiangxi Province Patentee after: Jiangxi Ganfeng Lithium Industry Group Co.,Ltd. Address before: 338000 Longteng Road, Xinyu Economic Development Zone, Jiangxi Province Patentee before: JIANGXI GANFENG LITHIUM Co.,Ltd. |
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| CP01 | Change in the name or title of a patent holder |