CN110230917A - Device for drying anhydrous lithium iodide and preparation method of anhydrous lithium iodide - Google Patents
Device for drying anhydrous lithium iodide and preparation method of anhydrous lithium iodide Download PDFInfo
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- CN110230917A CN110230917A CN201910520673.2A CN201910520673A CN110230917A CN 110230917 A CN110230917 A CN 110230917A CN 201910520673 A CN201910520673 A CN 201910520673A CN 110230917 A CN110230917 A CN 110230917A
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- lithium iodide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/04—Halides
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/04—Heating arrangements using electric heating
- F26B23/06—Heating arrangements using electric heating resistance heating
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention relates to a device for drying anhydrous lithium iodide and a preparation method of the anhydrous lithium iodide. According to the invention, the flask is a three-mouth round-bottom glass flask, lithium iodide trihydrate is subjected to vacuum drying in the flask, so that the cost is reduced, and the quick connectors are arranged among the flask, the vacuum pump and the argon bottle, so that the preparation process is more convenient and faster; the anhydrous lithium iodide prepared by the method effectively reduces the content of free iodine, so that the content of water and the content of free iodine both reach the quality requirement and are lower than 0.02 percent.
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a device for drying anhydrous lithium iodide and a preparation method of the anhydrous lithium iodide.
Background
The anhydrous lithium iodide is a fuel cell additive, the fuel cell is the most promising automobile power cell, and is also an electrolyte of a lithium-iron sulfide cell, the lithium-iron sulfide cell is a novel high-energy lithium cell, the capacity of the lithium-iron sulfide cell taking the lithium iodide as the electrolyte is 8 times higher than that of the common alkali manganese cell, the weight of the lithium-iron sulfide cell is only one half of that of the alkali manganese cell of the same type, and the voltage of the lithium-iron sulfide cell is 1.5V, so that the lithium-iron sulfide cell can directly replace the zinc manganese cell. It can be said that lithium-iron sulfide batteries are the most promising batteries for development. Lithium iodide single crystal is the most suitable crystal for slow neutron detector, and is widely used as a catalyst with high yield, stable reaction and good selectivity in organic synthesis.
The lithium ion battery electrolyte has high requirements on the purity of lithium iodide, and particularly has strict requirements on the moisture content. Because lithium iodide is very easy to absorb moisture, the third crystal water can be lost only at the temperature of over 300 ℃, and thus, the high-temperature lithium iodide is oxidized by oxygen in the air to free iodine, so how to completely remove the crystal water of the lithium iodide is a difficulty in developing anhydrous lithium iodide at present. The method for preparing anhydrous lithium iodide mainly comprises an organic solvent method, wherein lithium iodide with crystal water is dissolved in an organic solvent which is several times of the lithium iodide, and the principle that water and the organic solvent form a constant boiling point compound is utilized, so that water of the lithium iodide is taken out when the organic solvent is evaporated. A two-stage pump air-pumping high-vacuum degree method is characterized in that a first-stage oil diffusion pump or a molecular pump is added on the basis of a rotary-vane vacuum pump, equipment is complex, and industrial large-scale production cannot be realized. And a hydrogen iodide atmosphere protection method is adopted, and the method has the defects of high operation difficulty and environmental pollution.
The present invention has been made in view of the above circumstances.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a device for drying anhydrous lithium iodide and a preparation method of the anhydrous lithium iodide.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a device of dry anhydrous lithium iodide, includes electric jacket, flask, vacuum pump, argon gas bottle and vacuum pressure table, the flask set up inside the electric jacket, the flask be three-necked flask, three mouth is first interface, second interface and third interface respectively, first interface, second interface and third interface respectively through pipeline and argon gas bottle, vacuum pressure table and vacuum pump sealing connection.
Furthermore, a thermometer for measuring the internal temperature of the flask is connected to the second interface.
Furthermore, the first interface and the third interface are respectively connected with a joint for controlling the flask to be communicated or disconnected with the argon bottle and the vacuum pump.
Furthermore, the joint is a quick joint, one side of the quick joint is connected with the flask, and the other side of the quick joint is connected with the pipeline.
Furthermore, a spring valve for controlling the quick connector to open and close is arranged in one side of the quick connector connected with the flask.
The electric heating jacket adopts the temperature-control constant-temperature electric heating jacket, can control the heating temperature of the electric heating jacket to be constant, and ensures that the temperature is favorable for reaction.
A method for preparing anhydrous lithium iodide by using the device comprises the following steps:
(1) Putting lithium iodide trihydrate into a flask, connecting the devices, vacuumizing the flask for 8-12min, slowly heating to 78-82 ℃ through an electric heating jacket, and drying;
(2) And continuously heating to 240-260 ℃, drying, closing the electric heating sleeve, naturally cooling to room temperature, closing the vacuum pump, introducing argon, closing the spring valve, taking down the flask, transferring into a glove box, and taking out anhydrous lithium iodide.
Further, in the step (1), drying is carried out for 1.5-2.5 hours.
Further, argon gas is introduced every 30min during the drying in the step (1).
Further, the drying time in the step (2) is 6 to 10 hours.
Further, argon gas is introduced every 30min during the drying in the step (2).
The heating rate in the invention is controlled at 0.5 ℃/min, and the purity of argon is 99.99%.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the flask is a three-mouth round-bottom glass flask, lithium iodide trihydrate is subjected to vacuum drying in the flask, so that the cost is reduced, and the quick connectors are arranged among the flask, the vacuum pump and the argon bottle, so that the preparation process is more convenient and faster;
(2) According to the invention, the vacuum drying is carried out under the protection of high vacuum and argon gas, so that the oxidative decomposition of lithium iodide is prevented, argon gas with the purity of 99.99% is introduced in the drying process, the drying efficiency is improved, lithium iodide is protected by inert gas, and the product is prevented from being oxidized;
(3) The anhydrous lithium iodide prepared by the method effectively reduces the content of free iodine, so that the content of water and the content of free iodine both meet the quality requirement, the drying temperature does not need to be too high to meet the quality requirement, and the content of water and the content of free iodine both are lower than 0.02 percent after the lithium iodide trihydrate is dehydrated.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of the structure of an apparatus for drying anhydrous lithium iodide according to the present invention;
reference numerals
1-electric heating jacket, 2-flask, 21-first interface, 22-second interface, 23-third interface, 3-quick joint, 4-vacuum pump, 5-vacuum pressure gauge, 6-thermometer and 7-argon bottle.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
As shown in fig. 1, the device for drying anhydrous lithium iodide of this embodiment includes an electric jacket 1, a flask 2, a vacuum pump 4, an argon gas bottle 7 and a vacuum pressure gauge 5, the flask 2 is disposed inside the electric jacket 1, the flask 2 is a three-neck flask, the three necks are respectively a first joint 21, a second joint 22 and a third joint 23, and the first joint 21, the second joint 22 and the third joint 23 are respectively connected with the argon gas bottle 7, the vacuum pressure gauge 5 and the vacuum pump 4 in a sealing manner through pipelines.
In a further scheme, the second interface 22 is also connected with 6 for measuring the internal temperature of the flask. The first interface 21 and the third interface 23 are respectively connected with joints for controlling the flask 2 to be communicated with or disconnected from the argon bottle 7 and the vacuum pump 4. The joint is a quick joint 3, one side of the quick joint 3 is connected with the flask 2, and the other side of the quick joint is connected with a pipeline. And a spring valve for controlling the quick connector to open and close is arranged in one side of the quick connector 3 connected with the flask 2.
The quick coupling 3 of the present invention is made by the prior art, and the specific structure is not within the protection scope of the present invention. The whole device for drying the anhydrous lithium iodide is a sealed device, three interfaces of the flask 2 are connected with other structures through rubber stoppers, so that the flask 2 can be ensured to be in a sealed state, lithium iodide trihydrate is firstly added into the flask 2 in the whole drying process, and then the other structures are assembled according to the scheme shown in figure 1 to form a complete drying device.
Example 2
This example is a process for preparing anhydrous lithium iodide using the apparatus of example 1, comprising the steps of:
(1) Putting 500g of lithium iodide trihydrate into a 5000ml three-neck flask, connecting the devices, vacuumizing the flask for 8min, slowly heating to 78 ℃ through an electric heating jacket while vacuumizing, and drying for 2.5h, wherein the heating rate is controlled at 0.5 ℃/min, and argon is introduced every 30min in the drying process;
(2) And (3) continuing vacuum drying, then heating to 240 ℃, drying for 10 hours again, controlling the heating rate at 0.5 ℃/min, introducing argon every 30min in the drying process, closing the electric heating sleeve, stopping heating, continuing to maintain vacuumizing, waiting for the flask to be naturally cooled to room temperature, introducing argon, closing a spring valve on the flask, taking down the flask, transferring into a glove box, and taking out anhydrous lithium iodide.
Example 3
This example is a process for preparing anhydrous lithium iodide using the apparatus of example 1, comprising the steps of:
(1) Putting 500g of lithium iodide trihydrate into a 5000ml three-neck flask, connecting the devices, vacuumizing the flask for 10min, slowly heating to 80 ℃ through an electric heating jacket while vacuumizing, and drying for 2h, wherein the heating rate is controlled at 0.5 ℃/min, and argon is introduced every 30min in the drying process;
(2) And (3) continuing vacuum drying, then heating to 250 ℃, drying for 8 hours, controlling the heating rate at 0.5 ℃/min, introducing argon every 30min in the drying process, closing the electric heating sleeve, stopping heating, continuing to maintain vacuumizing, waiting for the flask to be naturally cooled to room temperature, introducing argon, closing a spring valve on the flask, taking down the flask, transferring into a glove box, and taking out anhydrous lithium iodide.
Example 4
This example is a process for preparing anhydrous lithium iodide using the apparatus of example 1, comprising the steps of:
(1) Putting 1000g of lithium iodide trihydrate into a 5000ml three-neck flask, connecting the devices according to the devices, vacuumizing the flask for 10min, slowly heating to 80 ℃ through an electric heating jacket while vacuumizing, drying for 2h, controlling the heating rate at 0.5 ℃/min, and introducing argon every 30min in the drying process;
(2) And (3) continuing vacuum drying, then heating to 250 ℃, drying for 10 hours again, controlling the heating rate at 0.5 ℃/min, introducing argon every 30min in the drying process, closing the electric heating sleeve, stopping heating, continuing to maintain vacuumizing, waiting for the flask to be naturally cooled to room temperature, introducing argon, closing a spring valve on the flask, taking down the flask, transferring into a glove box, and taking out anhydrous lithium iodide.
Example 5
This example is a process for preparing anhydrous lithium iodide using the apparatus of example 1, comprising the steps of:
(1) Putting 1000g of lithium iodide trihydrate into a 5000ml three-neck flask, connecting the devices according to the devices, vacuumizing the flask for 12min, slowly heating to 78 ℃ through an electric heating jacket while vacuumizing, and drying for 2.5h, wherein the heating rate is controlled at 0.5 ℃/min, and argon is introduced every 30min in the drying process;
(2) And continuously drying in vacuum, heating to 260 ℃, drying for 6 hours again, controlling the heating rate at 0.5 ℃/min, introducing argon every 30min in the drying process, closing the electric heating sleeve, stopping heating, continuously keeping vacuumizing, waiting for the flask to be naturally cooled to room temperature, introducing argon, closing a spring valve on the flask, taking down the flask, transferring the flask into a glove box, and taking out anhydrous lithium iodide.
Test example 1
The water content and the free iodine content of each of the lithium iodide sewage prepared in examples 2 to 5 were measured, and the results are shown in Table 1.
TABLE 1
| Test sample | Moisture content (%) | Free iodine content (%) |
| Example 2 | 0.012 | 0.006 |
| Example 3 | 0.010 | 0.008 |
| Example 4 | 0.009 | 0.011 |
| Example 5 | 0.012 | 0.013 |
Test example 2
The influence of the drying temperature on the moisture and free iodine content of the prepared anhydrous lithium iodide was investigated.
Anhydrous lithium iodide was prepared according to the method of example 3, except that the drying temperature in step (2) was changed and the conditions were the same, and the influence of moisture and free iodine content in anhydrous lithium iodide at different temperatures was investigated, and the results are shown in table 2.
TABLE 2
| Temperature (. Degree.C.) | Moisture content (%) | Free iodine content (%) |
| 230 | 1.21 | 0.004 |
| 235 | 0.68 | 0.006 |
| 240 | 0.018 | 0.007 |
| 250 | 0.010 | 0.008 |
| 260 | 0.0089 | 0.011 |
| 265 | 0.0076 | 0.069 |
| 275 | 0.0069 | 0.098 |
It can be seen from table 2 that, in the drying temperature range of the present invention, the moisture content and the free iodine content both meet the quality requirement, the temperature is too low, the moisture content is high, the temperature is too high, and the free iodine content is too high, which is because the crystal water on the lithium iodide trihydrate cannot be separated at the too low temperature, and the lithium iodide is oxidized into free iodine at the too high temperature, and the anhydrous lithium iodide prepared by the apparatus of the present invention can be prepared at 240-260 ℃ because of the closed apparatus and the protection of argon gas.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The utility model provides a device of dry anhydrous lithium iodide, its characterized in that, includes electric jacket, flask, vacuum pump, argon gas bottle and vacuum pressure table, the flask set up inside the electric jacket, the flask be three-neck flask, three mouth is first interface, second interface and third interface respectively, first interface, second interface and third interface respectively through pipeline and argon gas bottle, vacuum pressure table and vacuum pump sealing connection.
2. The apparatus of claim 1, wherein said second port is further connected to a thermometer for measuring the temperature inside the flask.
3. The apparatus for drying anhydrous lithium iodide as claimed in claim 1, wherein the first port and the third port are respectively connected with a connector for controlling the connection or disconnection of the flask with the argon bottle and the vacuum pump.
4. The apparatus of claim 3, wherein the connector is a quick connector, and one side of the quick connector is connected to the flask and the other side of the quick connector is connected to a pipeline.
5. The apparatus for drying anhydrous lithium iodide as claimed in claim 4, wherein a spring valve is provided in the side of the quick coupling connected to the flask for controlling the opening and closing of the quick coupling.
6. A method for preparing anhydrous lithium iodide using the apparatus of any one of claims 1 to 5, comprising the steps of:
(1) Putting lithium iodide trihydrate into a flask, connecting the devices, vacuumizing the flask for 8-12min, slowly heating to 78-82 ℃ through an electric heating jacket, and drying;
(2) And continuously heating to 240-260 ℃, drying, closing the electric heating sleeve, naturally cooling to room temperature, closing the vacuum pump, introducing argon, closing the spring valve, taking down the flask, transferring into a glove box, and taking out anhydrous lithium iodide.
7. The process for preparing anhydrous lithium iodide as claimed in claim 6, wherein the drying in step (1) is carried out for 1.5 to 2.5 hours.
8. The method of claim 7, wherein the step (1) of drying is performed by passing argon gas every 30 min.
9. The process for preparing anhydrous lithium iodide as claimed in claim 6, wherein the drying time in the step (2) is 6 to 10 hours.
10. The method of claim 9, wherein the step (2) of drying is performed by passing argon gas every 30 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111579416A (en) * | 2020-06-09 | 2020-08-25 | 湖北百杰瑞新材料股份有限公司 | Water content detection method of anhydrous lithium iodide |
| CN112739971A (en) * | 2020-06-05 | 2021-04-30 | 广州理文科技有限公司 | Device and method for drying lithium battery electrolyte assisted by ultrasonic waves |
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Application publication date: 20190913 |