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Preparation and comprehensive utilization method of magnesium bicarbonate solution

A technology of magnesium bicarbonate and solution, applied in the direction of magnesium carbonate, chemical instruments and methods, magnesium halide, etc., can solve the problems of high production cost, low magnesium calcium carbonate, cost increase, etc., achieve good economic and social benefits, promote Crystal nucleation growth, effect of improving filtration performance

Active Publication Date: 2013-11-06
GRIREM ADVANCED MATERIALS CO LTD
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  • Abstract
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Problems solved by technology

The main problems in this process: ① A large amount of low-value magnesium-containing calcium carbonate is produced. If it is not recycled, about 5.5 tons of magnesium-containing calcium carbonate with a net weight of about 5.5 tons per ton of light magnesium oxide will be discharged to form a paste (nearly 10 tons of waste residue). Cause environmental pollution and waste of resources
②The magnesium oxide content in the heavy magnesium water obtained by the dolomite carbonization method is low, and the water consumption is large, resulting in pyrolysis energy consumption accounting for more than 40% of the total energy consumption, and the production cost is high
The above-mentioned rare earth solutions are usually precipitated with oxalic acid and roasted to obtain rare earth oxides. The product obtained by this method has high purity, but oxalic acid is expensive, the production cost is high, and a large amount of oxalic acid wastewater is produced; some products use ammonia water or ammonium bicarbonate as a precipitant to produce rare earth Carbonates or hydroxides can also be roasted to obtain rare earth oxides, but a large amount of ammonia nitrogen wastewater is produced to pollute the environment. The cost of recycling ammonia nitrogen wastewater is very high, and it is difficult to meet the requirements of environmental protection standards; some companies use sodium carbonate in order to eliminate ammonia nitrogen wastewater pollution. Instead of ammonium bicarbonate or ammonia as a precipitant to produce rare earth carbonates or oxides, but the cost is doubled, and it also brings sodium salt wastewater pollution

Method used

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  • Preparation and comprehensive utilization method of magnesium bicarbonate solution

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Roast the dolomite at 1000°C for 4 hours to obtain calcium oxide and magnesium oxide powder. Take 915g (CaO content of 60wt%) and add it to 5L magnesium chloride solution (2mol / L). The amount of calcium oxide in the added powder is oxidized in the magnesium chloride solution. The molar ratio of magnesium is CaO / MgO=98%, the reaction is stirred for 1 hour, the pH is 10.4, clarified and filtered, and the filtration time is 10 minutes, and then washed to obtain 2198g of magnesium hydroxide filter cake and calcium chloride filtrate. The filtrate is concentrated, Crystallize, filter, and dry to obtain 1368g of calcium chloride dihydrate by-product, with CaCl 2 The total content is 69.3%, reaching industrial-grade qualified products.

[0047] After the magnesium hydroxide filter cake is washed with calcium, the molar ratio of CaO / MgO in the filter cake is tested to be 0.8%. It is slurried with water to 12g / L (calculated as MgO), and then 80V% carbon dioxide gas is introduced into...

Embodiment 2

[0052] Roast the dolomite at 1150℃ for 4h to obtain 420kg of calcium oxide and magnesium oxide powder (CaO content is 60wt%), slowly add it to 4.2m 3 In the 1.2mol / L magnesium chloride solution, the molar ratio of the amount of calcium oxide in the powder to the amount of magnesium oxide in the magnesium chloride solution is CaO / MgO=90%, the pH of the reaction is 9.8, and then filtered and washed to obtain the magnesium hydroxide filter Cake 1262kg and calcium chloride filtrate, the filtrate is heated and concentrated to obtain 628.5kg of calcium chloride dihydrate by-product, with CaCl 2 The total content is 60.5%.

[0053] After the magnesium hydroxide filter cake is washed with calcium, the molar ratio of CaO / MgO in the filter cake is tested to be 0.1%, and the water is adjusted to 25g / L (MgO meter), and then 50V% carbon dioxide gas (kiln gas) is introduced into the magnesium hydroxide slurry. Mixed with CO produced during precipitation 2 (Gas) to a partial pressure of 0.4MPa, ...

Embodiment 3

[0056] Roast the dolomite at 950°C for 10 hours to obtain 1367g of calcium oxide and magnesium oxide powder (CaO content is 59wt%), which is mixed with 7.7L of 1.95mol / L magnesium chloride solution for digestion and alkali conversion. The amount of calcium oxide in the added powder The molar ratio CaO / MgO to the amount of magnesium oxide in the magnesium chloride solution is CaO / MgO=96%, and the pH of the reaction is 10.2, then filtered and washed to obtain 3662g of magnesium hydroxide filter cake and calcium chloride filtrate. The filtrate is heated and concentrated to obtain dihydrate chlorine Calcium by-product 2011g, with CaCl 2 The total content is 69.0%, reaching industrial-grade qualified products.

[0057] After the magnesium hydroxide filter cake was washed with calcium, the molar ratio of CaO / MgO in the filter cake was tested to be 0.5%. It was slurried with water to 9.1g / L (calculated as MgO), and then the magnesium hydroxide slurry was passed into 35V% carbon dioxide g...

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Abstract

The invention relates to a preparation and comprehensive utilization method of a magnesium bicarbonate solution. The method is used to prepare the magnesium bicarbonate solution used for deposition, crystallization and recovery of rare earth ions, and comprehensive recovery of calcium-compound products and magnesium-compound products by taking dolomite as a raw material. The method specifically comprises: roasting dolomite to obtain a powder containing calcium oxide and magnesium oxide, directly mixing with a magnesium chloride solution for digestion and alkali transformation at the same time to prepare a magnesium hydroxide secondary-product and a calcium compound secondary-product, and further to realize effective separation of calcium and magnesium; performing slurry mixing on magnesium hydroxide, introducing carbon dioxide gas for a carbonization reaction to prepare the magnesium bicarbonate solution; applying obtained magnesium bicarbonate to deposition and crystallization of the rare earth ions to produce rare-earth carbonate or rare-earth oxide products; and recycling one part of the filtrate to prepare magnesium bicarbonate, and evaporating one part of the filtrate for crystallization to produce the magnesium compound product.

Description

Technical field [0001] The invention relates to a method for the preparation and comprehensive utilization of a magnesium bicarbonate solution. Specifically speaking, dolomite is used as raw material to prepare pure magnesium bicarbonate solution, which is used for the precipitation and crystallization of rare earth ions to produce rare earth carbonate or oxide products, while comprehensively recovering calcium and magnesium products, which belongs to the field of comprehensive utilization of dolomite. Background technique [0002] Dolomite is a natural mineral composed of calcium carbonate and magnesium carbonate, generally white, off-white and yellow. The chemical formula is CaMg(CO 3 ) 2 , The theoretical molar ratio of calcium to magnesium is roughly 1:1; it also contains a small amount of calcite CaCO 3 And a very small amount of quartz SiO 2 Wait. my country's dolomite resources are very rich and widely distributed. The production areas are all over the country. The main p...

Claims

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Application Information

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IPC IPC(8): C01F5/24C01F5/30C01F17/00C01F11/24C01F11/46C01B7/01
Inventor 黄小卫冯宗玉王猛龙志奇于赢侯永可崔梅生
Owner GRIREM ADVANCED MATERIALS CO LTD
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