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Method for preparing anhydrous magnesium chloride by utilizing magnesium chloride hexahydrate

A technology of magnesium chloride hexahydrate and anhydrous magnesium chloride, which is applied in the direction of magnesium chloride and magnesium halide, can solve the problems of low utilization rate of chlorine gas, easy blockage of pipelines, and large investment in tail gas treatment, so as to reduce environmental protection input costs, reduce production costs, shorten The effect of the production process

Active Publication Date: 2012-06-13
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the amount of ammonium chloride is too large, which makes the production cost high, and it is difficult to recover ammonium chloride in the production process and it is easy to block the pipeline
[0006] (4) Magnesium oxide chlorination to prepare anhydrous magnesium chloride method (IG Farben method), which is to react agglomerates of magnesium oxide and reducing agent carbon with chlorine gas in an electric heating shaft furnace (about 800 ° C) to prepare molten anhydrous magnesium chloride , its disadvantages are low production efficiency, low utilization rate of chlorine gas and large investment in tail gas treatment, and there are chlorinated hydrocarbons in the exhaust gas
Using gas chlorinating agent (HCl or Cl 2 ) In the melt, the preparation containing anhydrous magnesium chloride melt mainly has the following problems: a) the gas chlorination agent utilization rate is not high, because the gas is difficult to realize uniform dispersion in the melt, and needs to keep enough chlorine in the whole melt Magnesium oxide can be converted into magnesium chloride only when the gas concentration is reduced, especially when the magnesium oxide content in the melt is low, the gas chlorination agent utilization rate is very low; b) the recycling of the hydrochloric hydrogen gas obtained during dehydration requires a complex drying system, and this System cost and operating cost are high

Method used

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  • Method for preparing anhydrous magnesium chloride by utilizing magnesium chloride hexahydrate
  • Method for preparing anhydrous magnesium chloride by utilizing magnesium chloride hexahydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 17.7g of magnesium chloride hexahydrate and 2.4g of ammonium chloride were ball milled with a ball with a diameter of 10mm, the mass ratio of the ball to the solid material was 1:6, and after ball milling for 60 minutes, a mixture of ammonium carnallite and magnesium chloride hexahydrate was obtained. The mixture was kept at 160° C. for 3 hours to obtain a mixture of ammonium carnallite and magnesium chloride hexahydrate. The mixture was put into a 50ml crucible, and then 12g of quartz sand was covered on the carnallite material. Put the lid on the crucible and first keep it warm at 410°C for 1.5 hours, and then keep it warm at 700°C for 0.5 hour, so that the upper layer of quartz sand and the lower layer of anhydrous magnesium chloride with obvious stratification are obtained. In this embodiment, based on the addition of 1.00 parts by weight of magnesium chloride hexahydrate, the addition of quartz sand is 0.68 parts by weight, and the addition of ammonium chloride is 0...

Embodiment 2

[0044] 17.7g of magnesium chloride hexahydrate and 4.7g of ammonium chloride were ball milled with a ball with a diameter of 10mm, the mass ratio of the ball to the solid material was 1:6, and ammonium carnallite was obtained after ball milling for 60 minutes. Ammonium carnallite was kept at 160°C for 3 hours to obtain low-water ammonium carnallite (MgCl 2 ·NH 4 Cl nH 2 O, n=0.8), put the low-water ammonium carnallite into a 50ml crucible, then cover the low-water ammonium carnallite material with 12g of alumina, put the lid on the crucible and keep it warm at 250°C 1.5 hours, and then kept at 700°C for 0.5 hours, so that the upper layer of alumina and the lower layer of anhydrous magnesium chloride with obvious stratification were obtained. In this embodiment, based on the addition of 1.00 parts by weight of magnesium chloride hexahydrate, the addition of aluminum oxide is 0.68 parts by weight, and the addition of ammonium chloride is 0.27 parts by weight.

[0045] The obt...

Embodiment 3

[0050] 17.7g of magnesium chloride hexahydrate and 4.7g of ammonium chloride were ball milled with a ball with a diameter of 10mm, the mass ratio of the ball to the solid material was 1:6, and ammonium carnallite was obtained after ball milling for 60 minutes. Ammonium carnallite was kept at 160°C for 3 hours to obtain low-water ammonium carnallite (MgCl 2 ·NH 4 Cl nH 2 O, n=0.7), put the low-water ammonium carnallite into a 50ml crucible, then cover 12g of alumina on the low-water ammonium carnallite material, put the lid on the crucible and keep it warm at 300°C 1.5 hours, and then kept at 700°C for 0.5 hours, so that the upper layer of alumina and the lower layer of anhydrous magnesium chloride with obvious stratification were obtained. In this embodiment, based on the addition of 1.00 parts by weight of magnesium chloride hexahydrate, the addition of aluminum oxide is 0.68 parts by weight, and the addition of ammonium chloride is 0.27 parts by weight.

[0051] The obtai...

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Abstract

The invention relates to a method for preparing anhydrous magnesium chloride by utilizing magnesium chloride hexahydrate. The method comprises the following steps of (1) mixing and ball-milling the magnesium chloride hexahydrate and ammonium chloride to obtain ammonium camallite or mixture containing the ammonium camallite, (2) heating the mixture and performing preliminary dehydration to preparelower-water ammonium camallite or mixture containing the lower-water ammonium camallite, and (3) placing a covering on the product obtained in the step (2) and performing heating and reaction to prepare anhydrous magnesium chloride. The method for preparing the anhydrous magnesium chloride by utilizing the magnesium chloride hexahydrate can shorten production process of the anhydrous magnesium chloride, improve production efficiency and reduce production cost and input cost for environmental protection.

Description

technical field [0001] The invention relates to a preparation technology of anhydrous magnesium chloride, in particular to a method for preparing anhydrous magnesium chloride by using magnesium chloride hexahydrate. The anhydrous magnesium chloride prepared by the method can be directly used for producing metal magnesium by an electrolysis method. Background technique [0002] The key link in the production of metal magnesium by electrolytic magnesium chloride is the preparation of anhydrous magnesium chloride. The method for preparing anhydrous magnesium chloride has: [0003] (1) Low-water ammonium carnallite ammonia method to prepare anhydrous magnesium chloride. Yuichi Suzukaw described the specific operation process and principle of the method in the patent US3798314: first low water ammonium carnallite (MgCl 2 ·NH 4 Cl nH 2 O, n=0.5-4) is initially dehydrated at 110°C-160°C, and the product of the initial dehydration is reacted with ammonia gas at 200°C-400°C to fo...

Claims

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Application Information

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IPC IPC(8): C01F5/34
Inventor 卢旭晨张志敏
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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