CN1613770A - Process for producing anhydrous magnesium chloride by microwave energy - Google Patents
Process for producing anhydrous magnesium chloride by microwave energy Download PDFInfo
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- CN1613770A CN1613770A CN 200410041515 CN200410041515A CN1613770A CN 1613770 A CN1613770 A CN 1613770A CN 200410041515 CN200410041515 CN 200410041515 CN 200410041515 A CN200410041515 A CN 200410041515A CN 1613770 A CN1613770 A CN 1613770A
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Abstract
Anhydrous magnesium chloride production by microwave energy is disclosed. It is carried out by dehydrating hexhydrated magnesium chloride to obtain magnesium chloride with 1.5-2.0 water content in the first microwave heater, dehydrating hexhydrated magnesium chloride to obtain tetrahydrated magnesium chloride at temperature 100-120deg.C, dehydrating tetrahydrated magnesium chloride to obtain magnesium chloride with 1.5-2.0 water content at temperature 100-150deg.C, and realizing magnesium chloride with 1.5-2.0 water content to obtain anhydrous magnesium chloride at temperature 150-350deg.C. It achieves low dehydrating temperature and short time.
Description
Technical Field
The invention relates to a new production process, in particular to a new production process for preparing anhydrous magnesium chloride by microwave energy.
Background
Anhydrous magnesium chloride MgCl2Is an indispensable raw material for preparing metal magnesium by electrolysis. In the last decade, the use of bischofite MgCl has been increasing at a rate of about 5% per year due to the increasing demand for magnesium metal in both traditional industrial applications and new technology areas, such as the quantity of western magnesium metal increasing at a rate of about 5% per year2.6H2Preparation of high-purity anhydrous magnesium chloride MgCl from O2Has been the subject of intense research in various countries throughout the world for many years.
The existing preparation process of anhydrous magnesium chloride comprises the following steps of production, development and research:
1. in the presence of HCl and Cl2Dehydrating under atmosphere. Namely, the proper concentration of hydrogen chloride or chlorine gas is maintained in the reaction system at a certain temperature, so that the hydrolysis of magnesium chloride hexahydrate or bischofite during the heating and removing crystal water can be avoided or reduced to the minimum degree. Because the hydrogen chloride atmosphere needs high temperature of about 450 ℃, the energy consumption is large, the equipment is seriously corroded under the high-temperature operation, and the hydrolysis and the side reaction are easy to occur under the high temperature. Relatively low reaction temperature in the chlorine atmosphere, process operation control and environmental protectionIt is still necessary to perfect.
2. Double salt method process. Adding hydrated magnesium chloride MgCl2.6H2And reacting the O with potassium chloride or ammonium chloride to prepare potassium or ammonium carnallite with a double-salt structure, and heating to remove crystal water in the potassium or ammonium carnallite. Because the activity of magnesium chloride in carnallite is less than that of hydrated magnesium chloride, hydrolysis in the dehydration process is obviously reduced, and the quality of anhydrous magnesium chloride is improved, but the problems of large relative flux, high energy consumption, incapability of continuous production process in the electrolysis process, low recovery rate and the like exist.
3. Ammonia complexation dehydration method. The process is a key development approach at home and abroad. The technology adopts alcohol to replace crystal water and magnesium chloride to form a complex, removes the crystal water and then forms hexammine MgCl through ammoniation2.6NH3Calcining at 450 ℃ to obtain the anhydrous magnesium chloride. The operation condition is relatively mild, the yield of magnesium chloride is high, the content of hydrolysate in the product is low, the use amount of ammonia and organic solvent is low, the reaction crystal size is large, the filtering is easy, and the industrialization is favorably realized.
The application of microwave heating technology in the chemical and metallurgical fields has been greatly developed in the last two decades. The method can be used for preparing anhydrous magnesium chloride with good effect. Compared with the traditional heating mode, the microwave radiation heating has obvious advantages on the aspects of production efficiency, product quality, energy conservation, labor improvement, production conditions and the like. The characteristics of internal heating of microwave radiation, rapid heating, selective heating, controllability of a heating device, high-frequency vibration without a stirring device and the like have wide prospects in the field of hydrometallurgy.
Disclosure of Invention
The invention aims to: provides a newproduction process for preparing anhydrous magnesium chloride by microwave energy, which removes bischofite MgCl by microwave heating2.6H2Crystal water in O and inhibitThe production of hydrolysate, the energy consumption for preparing the anhydrous magnesium chloride and the consumption of auxiliary materials are reduced, and the production efficiency and the utilization rate of a production device are improved.
The technical solution of the invention is as follows: the new process is implemented in two parts, firstly, the magnesium chloride hexahydrate to the magnesium chloride containing 1.5 to 2.0 percent of water is realized in a first microwave heater; then the magnesium chloride containing water 1.5-2.0 to anhydrous magnesium chloride is realized in the second microwave heater.
Magnesium chloride hexahydrate or bischofite MgCl2.6H2And O is conveyed into the first microwave radiation heater by conveying equipment, the conveying equipment is made of a non-metal material, microwave radiation heating energy penetrates and directly acts on the polar molecular material, and the heating reaction process of the crystal water is as follows: ， i.e. the magnesium chloride hexahydrate is formed into MgCl tetrahydrate in steps during heating2.4H2O and MgCl dihydrate2.2H2O。
The heating temperature is controlled by a temperature measuring instrument in a segmented manner at 80-120 ℃ and 100-150 ℃, and the magnesium chloride dihydrate material is produced immediately and basically no hydrolysate is produced.
When the thickness of the heated material is constant in the microwave heating radiation field, the temperature gradient is notgenerated, the heating direction is consistent with the escape direction of water molecules, the heating efficiency can be obviously improved, the heating time is shortened, and the energy consumption is saved.
After the magnesium chloride dihydrate is formed, the magnesium chloride dihydrate is sent into a second microwave heater, a dehydrating agent is added and uniformly stirred, the dehydrating agent is added according to 1-10% of the weight of the magnesium chloride dihydrate material, the microwave radiation heater is relatively closed, chlorine gas covering the surface area of the material is introduced to form a protective atmosphere relatively isolated from air, all crystal water is removed, and the temperature is controlled within the range of 150-350 ℃.
Due to the addition of the dehydrating agent, the material MgCl which has weak microwave radiation response capability2.2H2The capacity of O to absorb microwave heat energy is rapidly increased, so that the material MgCl2.2H2Two crystal water in O is rapidly removed along with the reaction with the dehydrating agent and the temperature increase. On one hand, chlorine gas is added to form protective atmosphere around the materials, and on the other hand, once the hydrolysate is generated, the hydrolysate is reduced under the combined action of carbon dioxide and chlorine gas formed by the dehydrating agent.
The reaction process of finally forming the anhydrous magnesium chloride is as follows:
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in addition to the above reaction processes, there are also a variety of side reactions associated with the above.
The materials in the microwave resonant cavity are conveyed in a conveying or spiral conveying mode, two-stage or three-stage conveying can be adopted according to the temperature control range, the first microwave heater is provided with a water vapor discharging device, the second microwave heater is provided with a chlorine dehydrating agent adding device, a water and air discharging device and a chlorine recovering device.
The dehydrating agent may be amorphous carbon, activated carbon, wood carbon, carbon black, coke or graphite.
The invention has the following advantages: 1. the temperature of the tax water is low, the speed is high, the time is short, the materials can be selectively heated, the heat is saved obviously, the production efficiency is improved, the continuous operation is realized, and the cost is reduced. 2. The processing equipment is simple to process, convenient to maintain and operate, and capable of realizing industrial production.
Drawings
FIG. 1 is a process flow chart of the present invention
Detailed Description
Example 1:
1. 200 g of MgCl hexahydrate2.6H2Placing O in a microwave ovenIn a heater, open the container and stir, control the temperature to 100 ℃, the exhauster works, and after removing two crystal water, magnesium chloride tetrahydrate MgCl is formed2.4H2O; the temperature is then raised to 150 ℃ to form MgCl magnesium chloride dihydrate2.2H2O, the process time is 5 minutes.
2. Moving the magnesium chloride dihydrate into a closed microwave heater with an air inlet and an air outlet, adding dehydrating agent active carbon accounting for 5 percent of the weight of the materials at the moment, introducing chlorine covering the surface area of the materials, fully stirring, heating to 230 ℃, and carrying out the time process for 5 minutes to obtain the anhydrous magnesium chloride capable of being used for electrolysis, wherein the MgO of the magnesium oxide is less than 0.5 percent; h2O＜0.3％。
Example 2:
1. putting 500 g of magnesium chloride hexahydrate into a microwave heater with a scraper for stirring and conveying, heating to 100 ℃ by microwaves, simultaneously operating an exhaust fan, increasing the temperature to 150 ℃, and obtaining MgCl dihydrate after 5 minutes2.2H2O。
2. Feeding the magnesium chloride dihydrate into a tubular microwave heater with stirring, respectively adding 4.5 wt% of dehydrating agent charcoal and 20ml of chlorine gas, heating to 240 deg.C by microwave, and obtaining anhydrous magnesium chloride for electrolysis after 10 min, wherein the content of MgO is less than 0.5%; h2O＜0.2％。
Example 3:
1. putting 500 g of magnesium chloride hexahydrate into a semicircular microwave heater with a stirrer, heating to 100 ℃ by using microwaves, simultaneously operating an exhaust fan, raising the temperature to 150 ℃, and obtaining the magnesium chloride dihydrate after 5 minutes.
2. Feeding the magnesium chloride dihydrate into a tubular microwave heater with a stirrer, and respectively adding carbon accounting for 4.5 percent of the weight of the materials and 20ml of chlorine gas to obtain anhydrous magnesium chloride with the content of magnesium oxide being less than 0.4 percent after 10 minutes; h2O＜0.2％。
Claims (10)
1. Thenew production process of preparing anhydrous magnesium chloride by microwave energy is characterized by comprising the following steps: the new process is implemented in two parts, firstly, the magnesium chloride hexahydrate is dehydrated in a first microwave heater to obtain the magnesium chloride with the water content of 1.5-2.0; then dehydrating the magnesium chloride containing 1.5 to 2.0 percent of water in a second microwave heater to obtain anhydrous magnesium chloride.
2. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 1, wherein: the first microwave heater realizes the dehydration of magnesium chloride hexahydrate by stages to obtain magnesium chloride with the water content of 1.5-2.0, the temperature is controlled to be 80-120 ℃ to realize the dehydration of magnesium chloride hexahydrate to obtain magnesium chloride tetrahydrate, and the temperature is controlled to be 100-150 ℃ to realize the dehydration of magnesium chloride tetrahydrate to obtain magnesium chloride with the water content of 1.5-2.0.
3. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 1, wherein: the temperature of the second microwave heater is controlled at 150-2。
4. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 3, wherein: adding dehydrating agent into the second microwave heater, wherein the dehydrating agent accounts for 1-10% of the weight of the magnesium chloride containing 1.5-2.0% of water.
5. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 4, wherein: the dehydrating agent is amorphous carbon, activated carbon, charcoal, carbon black, coke or graphite.
6. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 3, wherein: chlorine gas is added into the second microwave heater to inhibit hydrolysis.
7. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 6, wherein: the addition amount of the chlorine is the amount covering the surface area of the magnesium chloride dihydrate material.
8. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 1, wherein: the first microwave heater adopts a conveyor belt conveying or spiral conveying mode, and adopts two-stage or three-stage conveying according to a temperature control range.
9. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 1, wherein: the first microwave heater is provided with a water vapor discharge device.
10. The new process for producing anhydrous magnesium chloride by microwave energy according to claim 1, wherein: the second microwave heater is provided with a chlorine and dehydrating agent adding device, a water and air discharging device and a chlorination recovery device.
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| CNB2004100415152A CN1295151C (en) | 2004-07-24 | 2004-07-24 | Process for producing anhydrous magnesium chloride by microwave energy |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254942B (en) * | 2008-04-07 | 2010-06-02 | 昆明理工大学 | Method for preparing high-purity anhydrous indium trichloride |
| CN103991886A (en) * | 2014-05-28 | 2014-08-20 | 石河子大学 | Preparation method of anhydrous magnesium chloride |
| CN104556156A (en) * | 2014-12-29 | 2015-04-29 | 中国天辰工程有限公司 | Preparation method of anhydrous magnesium chloride |
| CN107208287A (en) * | 2014-12-10 | 2017-09-26 | 联盟镁公司 | By the way that two hydrated magnesium chlorides to be dehydrated to the method to produce magnesium metal |
| CN107254335A (en) * | 2017-07-24 | 2017-10-17 | 中国科学院青海盐湖研究所 | The method of comprehensive utilization of industrial waste product |
| CN109053229A (en) * | 2018-08-29 | 2018-12-21 | 交城县金兰化工有限公司 | A kind of preparation method of anti-caking water soluble fertilizer |
| CN109095491A (en) * | 2018-08-29 | 2018-12-28 | 交城县金兰化工有限公司 | A kind of microwave dehydration method of the inorganic salts containing the crystallization water |
| CN117344351A (en) * | 2023-12-06 | 2024-01-05 | 北京道思克能源设备有限公司 | Metal magnesium and preparation method thereof |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4698761A (en) * | 1985-03-21 | 1987-10-06 | General Electric Company | Automatic tunnel detector for a self-propelled traction vehicle |
| DE69433408T2 (en) * | 1993-10-28 | 2004-10-14 | Australian Magnesium Operations Pty, Ltd. | WATER-FREE MAGNESIUM CHLORIDE |
| SK282092B6 (en) * | 1994-05-17 | 2001-10-08 | Noranda Mettalurgy Inc. | Preparation of anhydrous magnesium chloride-containing melts from hydrated magnesium chloride and production of magnesium metal |
| NO308352B1 (en) * | 1997-06-20 | 2000-09-04 | Norsk Hydro As | Process for producing anhydrous MgCl2 |
| CN1156398C (en) * | 2001-08-17 | 2004-07-07 | 华东理工大学 | Methodf or preparing anhydrous magnesium chloride |
| CN1412114A (en) * | 2001-10-08 | 2003-04-23 | 谷亮 | New process for preparing anhydrous magnesium chloride |
| CN1234608C (en) * | 2002-01-01 | 2006-01-04 | 中国科学院青海盐湖研究所 | Method of preparing anhydrous magnesium chloride by dehydration of bischefite |
-
2004
- 2004-07-24 CN CNB2004100415152A patent/CN1295151C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254942B (en) * | 2008-04-07 | 2010-06-02 | 昆明理工大学 | Method for preparing high-purity anhydrous indium trichloride |
| CN103991886A (en) * | 2014-05-28 | 2014-08-20 | 石河子大学 | Preparation method of anhydrous magnesium chloride |
| CN107208287A (en) * | 2014-12-10 | 2017-09-26 | 联盟镁公司 | By the way that two hydrated magnesium chlorides to be dehydrated to the method to produce magnesium metal |
| US10617995B2 (en) | 2014-12-10 | 2020-04-14 | Alliance Magnésium | Process for producing magnesium metal by dehydrating dihydrate magnesium chloride |
| CN104556156A (en) * | 2014-12-29 | 2015-04-29 | 中国天辰工程有限公司 | Preparation method of anhydrous magnesium chloride |
| CN107254335A (en) * | 2017-07-24 | 2017-10-17 | 中国科学院青海盐湖研究所 | The method of comprehensive utilization of industrial waste product |
| CN109053229A (en) * | 2018-08-29 | 2018-12-21 | 交城县金兰化工有限公司 | A kind of preparation method of anti-caking water soluble fertilizer |
| CN109095491A (en) * | 2018-08-29 | 2018-12-28 | 交城县金兰化工有限公司 | A kind of microwave dehydration method of the inorganic salts containing the crystallization water |
| CN117344351A (en) * | 2023-12-06 | 2024-01-05 | 北京道思克能源设备有限公司 | Metal magnesium and preparation method thereof |
| CN117344351B (en) * | 2023-12-06 | 2024-02-13 | 北京道思克能源设备有限公司 | Metal magnesium and preparation method thereof |
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| CN1295151C (en) | 2007-01-17 |
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