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Method for preparing high-purity magnesium oxide with serpentine as raw material

A technology of antigorite and magnesium oxide, applied in the direction of magnesium oxide, etc., can solve the problems of low recovery rate, long process, difficult separation of silica gel, etc., and achieve the effect of good effect, simple process and low cost

Inactive Publication Date: 2013-11-27
CHINA UNIV OF GEOSCIENCES (WUHAN)
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Problems solved by technology

[0006] Chinese patent 88109734.9 proposes a method for producing magnesium carbonate / or magnesium oxide and porous silicon dioxide using serpentine as a raw material. The method is first calcined at 400-800°C for 2-4 hours, and then treated with inorganic acid for separation. This patent considers the possibility of efficiently recovering magnesium from serpentine magnesium-containing leaching solution, but these processes do not consider the leaching rate of magnesium enough, especially under simple normal temperature and pressure, it is difficult to leach valuable metals in silicates. It will inevitably lead to unsatisfactory leaching effect of target metals such as magnesium. In this patent, Mg 2+ The leaching rate can only reach more than 85%, and the above-mentioned patent uses sulfuric acid as a solvent for extraction, which will generate calcium sulfate precipitates, resulting in incomplete decomposition of mineral powder, and the formed silica gel is also difficult to separate
[0007] Chinese patent 89106821.X proposes a comprehensive utilization process of serpentine tailings. In the process of neutralization, milk of lime is used as a neutralizing agent, which allows a large amount of calcium oxide to be mixed into the magnesium chloride solution while removing iron. Ca in MgO 2+ Content is one of the most important indicators to measure product quality, and in the carbonization process, this method is the same as the traditional dolomite method to produce magnesium oxide, using CO 2 In the two-step method, it has been proved impossible to completely separate calcium and magnesium in the carbonization process. In addition, this method has a long process, low recovery rate, and serious pollution of chloride ions washed away.

Method used

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  • Method for preparing high-purity magnesium oxide with serpentine as raw material
  • Method for preparing high-purity magnesium oxide with serpentine as raw material
  • Method for preparing high-purity magnesium oxide with serpentine as raw material

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Place the antigorite ore powder ground to 200 mesh in a muffle furnace at 900°C for calcination for 60 minutes, weigh 20 g and add 200 mL of 50wt% hydrochloric acid, reflux and stir at 60°C for 50 minutes, and collect the filtrate by suction filtration after the reaction is completed. to contain Ca 2+ , Fe 3+ Magnesium salt solution such as impurity ions, add NH to the filtrate at room temperature 4 HCO 3 , adjust the pH to 8, let stand and age for 20 minutes, wait for the precipitate to gather into large particles, then go to suction filtration, wash the precipitate with water several times before suction filtration, in order to minimize the Mg adsorbed on the precipitate 2+ , the filtrate was heated in a water bath at 25°C, and NH was gradually added to the filtrate 4 HCO 3 , and finally the basic magnesium carbonate solid can be obtained, and the dried basic magnesium carbonate is put into a muffle furnace at 800°C for 3 hours to be pyrolyzed to obtain high-purit...

Embodiment 2

[0036] Put antigorite ore powder ground to 200 mesh in a muffle furnace at 800°C for calcination for 60 minutes, take 20g of antigorite ore powder activated by the above-mentioned calcination, add 200mL of 50wt% hydrochloric acid, and heat in a water bath at 60°C Reflux and stir for 50 minutes under the same conditions, and the other steps and process conditions are the same as in Example 1, and MgO with a leaching rate of 93.53% and a purity of 99.76% can be produced.

[0037] X-ray diffraction was done on the prepared MgO. The experimental conditions were Cu target Kα ray, Ni filter, wavelength 0.15406nm, tube pressure 40KV, scan rate 0.05° / s, scan interval 5°-70°; attached figure 2The characteristic peaks of the shown XRD pattern are consistent with the characteristic peaks of magnesium oxide, which indicates that the product obtained by this method is magnesium oxide, and no other impurity peaks appear, and the purity of the sample is high.

[0038] The magnesium oxide pr...

Embodiment 3

[0040] Put antigorite ore powder ground to 200 mesh in a muffle furnace at 700°C for 120 minutes and calcinate for 120 minutes, take 20 g of antigorite ore powder activated by the above-mentioned calcination, add 200mL of 50wt% hydrochloric acid, and heat at 20°C Stir for 20min, collect the filtrate by suction filtration after the reaction is completed, add NH to the filtrate at room temperature 4 HCO 3 , adjust the pH to 9, let stand and age for 10 minutes, wait for the precipitate to aggregate into large particles, then go to suction filtration, heat the filtrate in a water bath at 10°C, and gradually add NH to the filtrate 4 HCO 3 , and finally the basic magnesium carbonate solid can be obtained, and the dried basic magnesium carbonate is put into a muffle furnace at 700°C for pyrolysis for 2 hours.

[0041] MgO with a leaching rate of 93.4% and a purity of 98.39wt% was obtained.

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Abstract

The invention relates to a method for preparing high-purity magnesium oxide with serpentine as a raw material. The method specifically comprises the steps that: (1) serpentine is crushed, and is activated by calcining; (2) 50wt% of hydrochloric acid is added to the calcined and activated mineral powder for carrying out acid leaching; heating, refluxing, and stirring are carried out; pump filtration is carried out, and a filtrate is collected; (3) ammonium bicarbonate is added and a pH value is regulated to 8-9; the mixture is settled and aged for 10-30min; pump filtration is carried out, and filtrate is collected; and (4) ammonium bicarbonate is continued to be added into the filtrate, until no precipitate is formed; a reaction is carried out under a temperature of 10-30 DEG C, such that basic magnesium carbonate can be obtained; bake-drying and pyrolysis are carried out, such that high-purity magnesium oxide is obtained. The method provided by the invention has the advantages of simple process, low cost, and suitability for industrialized productions. With the calcining activation method, difficulty for removing iron ions and a small amount of calcium component from a high-content magnesium salt of a traditional chemical purification method is solved. Leaching rate of magnesium oxide in serpentine can be higher than 93.53%, and magnesium oxide purity can be higher than 99.78wt%.

Description

technical field [0001] The invention relates to a preparation method of magnesium oxide, in particular to a method for preparing high-purity magnesium oxide by using antigorite as a raw material. Background technique [0002] Serpentine is an alteration product of olivine, which is a general term for a hydrous magnesium-rich silicate mineral with the general formula Mg 3 Si 2 o 5 (OH) 4 , whose structure is a 1:1 layered silicate mineral composed of silicon-oxygen tetrahedron and magnesium hydroxide octahedron. According to the shape of its internal structural layer, it is divided into lizardite, antigorite and chrysotile. The content of magnesium oxide in antigorite is generally more than 36%, and antigorite mineral resources in my country are very rich. The discovered mining areas include Jiangsu Donghai, Anhui Xiexian, Hubei Yichang, etc., and each mining area has an antigorite reserve. Both are above 500 million tons. [0003] As an important inorganic chemical prod...

Claims

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Application Information

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IPC IPC(8): C01F5/06
Inventor 范晓雅杨祥徐晓晴卿恩平陈红闯刘晓刚
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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