CN1295151C - 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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- CN1295151C CN1295151C CNB2004100415152A CN200410041515A CN1295151C CN 1295151 C CN1295151 C CN 1295151C CN B2004100415152 A CNB2004100415152 A CN B2004100415152A CN 200410041515 A CN200410041515 A CN 200410041515A CN 1295151 C CN1295151 C CN 1295151C
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- magnesium chloride
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- anhydrous magnesium
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- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000008569 process Effects 0.000 title abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000013078 crystal Substances 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 18
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 16
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims abstract description 15
- 229960002337 magnesium chloride Drugs 0.000 claims abstract description 14
- 239000012024 dehydrating agents Substances 0.000 claims abstract description 13
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 claims abstract description 11
- 239000000460 chlorine Substances 0.000 claims abstract description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 7
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 7
- XEEYVTMVFJEEEY-UHFFFAOYSA-L magnesium;dichloride;tetrahydrate Chemical compound O.O.O.O.[Mg+2].[Cl-].[Cl-] XEEYVTMVFJEEEY-UHFFFAOYSA-L 0.000 claims abstract 4
- DARFZFVWKREYJJ-UHFFFAOYSA-L magnesium dichloride dihydrate Chemical compound O.O.[Mg+2].[Cl-].[Cl-] DARFZFVWKREYJJ-UHFFFAOYSA-L 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 229910003481 amorphous carbon Inorganic materials 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000000571 coke Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 24
- 230000001681 protective effect Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000005855 radiation Effects 0.000 description 6
- 239000000413 hydrolysate Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229940091250 magnesium supplement Drugs 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明公开了微波能制取无水氯化镁生产工艺，该工艺分二部分实施，首先在第一微波加热器内实现六水氯化镁脱水得含有1.5-2.0个结晶水的氯化镁，温度控制在100-120℃由六水氯化镁脱水得四化氯化镁，温度控制在120℃以上到150℃从四水氯化镁脱水得含有1.5-2.0个结晶水的氯化镁；然后在第二微波加热器内实现含水1.5-2.0氯化镁得无水氯化镁，温度控制在150-350℃，加入1-10%的脱水剂，保护气氛的氯气加入量为覆盖物料表面积用量。本发明采用微波能加热，脱水温度低，时间短，速率高，选择性加热节能显著，实现工业化连续作业，生产效率高。
The invention discloses a production process for producing anhydrous magnesium chloride by microwave energy. The process is implemented in two parts. Firstly, magnesium chloride hexahydrate is dehydrated in the first microwave heater to obtain magnesium chloride containing 1.5-2.0 crystal water, and the temperature is controlled at 100- Magnesium chloride tetrahydrate is dehydrated from magnesium chloride hexahydrate at 120°C, and magnesium chloride tetrahydrate is dehydrated from magnesium chloride tetrahydrate at a temperature controlled above 120°C to 150°C to obtain magnesium chloride containing 1.5-2.0 crystal water; Magnesium chloride is used to obtain anhydrous magnesium chloride, the temperature is controlled at 150-350°C, 1-10% of dehydrating agent is added, and the amount of chlorine added in the protective atmosphere is the amount used to cover the surface area of the material. The invention adopts microwave energy heating, low dehydration temperature, short time, high speed, remarkable energy saving in selective heating, realizes industrialized continuous operation, and high production efficiency.
Description
Technical Field
The invention relates to a production process, in particular to a 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 400 ℃, 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 at home and abroadThe pathway of (1). 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, rapid heating, selective heating, controllability of a heating device, high-frequency vibration without a stirring device and the like of microwave radiation have wide prospects in the field of hydrometallurgy.
Disclosure of Invention
The invention aims to: provides a production process for preparing anhydrous magnesium chloride by microwave energy, which removes bischofite MgCl by microwave heating2.6H2Crystal water and suppression of OThe hydrolysate is generated, 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 process is carried out in two parts, firstly, magnesium chloride hexahydrate to magnesium chloride containing 1.5-2.0 crystal water is realized in a first microwave heater; then removing residual crystal water in a second microwave heater to obtain the anhydrous magnesium chloride.
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 sections at 80-120 ℃ and above 120 ℃ to 150 ℃, and then the magnesium chloride dihydrate material is produced, 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 not generated, 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 response capability to microwave radiation2.2H2The capacity of O to absorbmicrowave heat energy is rapidly increased, so that the material MgCl2.2H2Two crystal water in O are rapidly removed along with the reaction of 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 monoxide 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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6、
7、
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19、
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 can be conveyed in two stages or three stages according to the temperature control range, the first microwave heater is provided with a water vapor discharge device, the second microwave heater is provided with a chlorine dehydrating agent adding device, a water and air discharge device and a chlorine recovery device.
The dehydrating agent may be amorphous carbon, activated carbon, charcoal, carbon black, coke or graphite.
The invention has the following advantages: 1. the dehydration temperature 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 diagram of the present invention
Detailed Description
Example 1:
1. 200 g of MgCl hexahydrate2.6H2The O is arranged in a microwave heater,opening the container and stirring, controlling the temperature to be 100 ℃, operating an exhauster, and removing two crystal waters to form MgCl tetrahydrate2.4H2O; 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 5.0 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 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. The magnesium chloride dihydrate is sent to a tubular microwave heater with stirring, 4.5 percent of dehydrating agent charcoal and 20ml of chlorine gas are respectively added in the weight of the materials,heating to 240 ℃ by microwave for 10 minutes to obtain anhydrous magnesium chloride for electrolysis, 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 (6)
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| Application Number | Priority Date | Filing Date | Title |
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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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| CNB2004100415152A CN1295151C (en) | 2004-07-24 | 2004-07-24 | Process for producing anhydrous magnesium chloride by microwave energy |
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| CN1613770A CN1613770A (en) | 2005-05-11 |
| CN1295151C true CN1295151C (en) | 2007-01-17 |
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| CN101254942B (en) * | 2008-04-07 | 2010-06-02 | 昆明理工大学 | Preparation method of high-purity anhydrous indium trichloride |
| CN103991886A (en) * | 2014-05-28 | 2014-08-20 | 石河子大学 | Preparation method of anhydrous magnesium chloride |
| WO2016090489A1 (en) | 2014-12-10 | 2016-06-16 | Alliance Magnésium | Process for producing magnesium metal by dehydrating dihydrate magnesium chloride |
| CN104556156B (en) * | 2014-12-29 | 2017-04-05 | 中国天辰工程有限公司 | A kind of preparation method of anhydrous magnesium chloride |
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| 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 |
| CN116282095B (en) * | 2023-01-12 | 2025-04-18 | 深圳市美凯特科技有限公司 | A kind of preparation method of anhydrous magnesium chloride |
| 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 |
| CN118767841B (en) * | 2024-08-06 | 2025-12-26 | 北京化工大学 | A process for preparing low-water materials using microwave-assisted catalytic dehydration reaction |
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| CN1333183A (en) * | 2001-08-17 | 2002-01-30 | 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 |
| CN1429770A (en) * | 2002-01-01 | 2003-07-16 | 中国科学院青海盐湖研究所 | Method of preparing anhydrous magnesium chloride by dehydration of bischefite |
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- 2004-07-24 CN CNB2004100415152A patent/CN1295151C/en not_active Expired - Fee Related
Patent Citations (7)
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| CN1003249B (en) * | 1985-03-21 | 1989-02-08 | 通用电气公司 | Automatic tunnel detector for a self-propelled traction vehicle |
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