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Preparation method of rhombohedral anhydrous magnesium carbonate

A technology of anhydrous magnesium carbonate and rhombohedron, applied in the direction of magnesium carbonate, etc., can solve the problems affecting the performance of processing technology and product performance, the increase of production cost, and the influence of product purity, so as to achieve easy control of production conditions, low production cost, The effect of complete crystal morphology

Active Publication Date: 2019-08-23
SHANDONG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis temperature of this method is high, the reaction time is long, and the production cost will increase accordingly; the obtained crystal plane is multi-layered and sawtooth stepped, and the shape is incomplete, and the surface will peel off during the process of mixing with other materials, which will affect other materials. Process performance and product performance
[0006] In summary, in the existing anhydrous magnesium carbonate synthetic method, or adopt solvothermal method or hydrothermal method to add chelating agent, both need to use organic additive, influence product purity and increase cost; Or only use magnesium salt and precipitation If the agent hydrothermal method is used, higher synthesis stability and longer synthesis time are required
At present, there are very few relevant research reports on the synthesis of rhombohedral anhydrous magnesium carbonate with a single phase, good dispersion, uniform particle size, and complete crystal morphology at low temperature and short time without using organic solvents and chelating agents.

Method used

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  • Preparation method of rhombohedral anhydrous magnesium carbonate
  • Preparation method of rhombohedral anhydrous magnesium carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) MgCl 2 ·6H 2 Add O into distilled water to prepare a transparent solution with a concentration of 0.1 mol / L, and use MgCl 2 ·6H 2 O and CH 4 N 2 The mass molar ratio of O is 1:8 by adding CH 4 N 2 O, stirred to obtain a transparent solution; MgCl 2 ·6H 2 O and CH 4 N 2 The solution prepared by O is heated to carry out pre-synthesis reaction, the reaction temperature is 95°C, and the reaction time is 1h;

[0022] (2) Transfer the mixed liquid after the pre-synthesis reaction to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction. The temperature of the hydrothermal reaction is 150°C, and the reaction time is 2h;

[0023] (3) After the hydrothermal reaction is completed, the product is filtered under negative pressure, washed and dried to obtain rhombohedral anhydrous magnesium carbonate.

[0024] According to X-ray diffraction analysis, anhydrous magnesium carbonate belongs to the trigonal crystal system ( figure 1 ), ...

Embodiment 2

[0026] (1) MgCl 2 ·6H 2 Add O into distilled water to prepare a transparent solution with a concentration of 0.2mol / L, and use MgCl 2 ·6H 2 O and CH 4 N 2 The mass molar ratio of O is 1:8 by adding CH 4 N 2 O, stirred to obtain a transparent solution; MgCl 2 ·6H 2 O and CH 4 N 2 The solution prepared by O is heated to carry out pre-synthesis reaction, the reaction temperature is 90°C, and the reaction time is 2h;

[0027] (2) Transfer the pre-synthesized mixed solution to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction, the temperature of the hydrothermal reaction is 140°C, and the reaction time is 4 hours;

[0028] (3) After the hydrothermal reaction is completed, the product is filtered under negative pressure, washed and dried to obtain rhombohedral anhydrous magnesium carbonate.

Embodiment 3

[0030] (1) MgCl 2 ·6H 2 Add O into distilled water to prepare a transparent solution with a concentration of 0.1 mol / L, and use MgCl 2 ·6H 2 O and CH 4 N 2The mass molar ratio of O is 1:8 by adding CH 4 N 2 O, stirred to obtain a transparent solution; MgCl 2 ·6H 2 O and CH 4 N 2 The solution prepared by O is heated to carry out pre-synthesis reaction, the reaction temperature is 80°C, and the reaction time is 2h;

[0031] (2) Transfer the mixed solution after the pre-synthesis reaction to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction. The temperature of the hydrothermal reaction is 145°C, and the reaction time is 3h;

[0032] (3) After the hydrothermal reaction is completed, the product is filtered under negative pressure, washed and dried to obtain rhombohedral anhydrous magnesium carbonate.

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Abstract

The invention provides a preparation method of rhombohedral anhydrous magnesium carbonate, and belongs to the technical field of inorganic chemical new materials. The preparation method comprises thefollowing steps: adding MgCl2.6H2O to distilled water to prepare a solution with a certain concentration, adding CH4N2O according to a certain mass molar ratio, and performing stirring to obtain a transparent solution; heating the prepared solution to carry out a pre-synthesis reaction at 80-95 DEG C for 1-2 h; transferring a mixed solution obtained after the pre-synthesis reaction into a stainless steel reactor with a polytetrafluoroethylene lining, and carrying out a hydrothermal reaction at 140-150 DEG C for 2-4 h; and carrying out negative pressure filtration, washing and drying on a product obtained after the hydrothermal reaction is completed in order to obtain the rhombohedral anhydrous magnesium carbonate. The rhombohedral anhydrous magnesium carbonate prepared in the present invention belongs to a trigonal system, the side length of every rhombus is 20-25 [mu]m, and the size of every rhombohedral particle is 25-30 [mu]m.

Description

technical field [0001] The invention relates to a preparation method of rhombohedral anhydrous magnesium carbonate, which belongs to the technical field of new inorganic chemical materials. Background technique [0002] Anhydrous magnesium carbonate is an important new inorganic chemical material, used as a pharmaceutical intermediate, antacid, desiccant, color-protecting agent, carrier, anti-caking agent, etc.; used as an additive and magnesium element compensator in food; Used as flame retardant, reinforcing agent, and filler in plastics and rubber; used in the manufacture of fire-resistant coatings, ink fillers, friction agents for toothpaste, etc. Different application fields have different requirements on the morphology and particle size uniformity of anhydrous magnesium carbonate, both of which will have a direct impact on its application fields and effects. [0003] At present, the synthesis methods of anhydrous magnesium carbonate mainly include: carbonization metho...

Claims

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Application Information

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IPC IPC(8): C01F5/24
CPCC01F5/24C01P2002/72C01P2004/03
Inventor 李国昌李成峰孙海滨
Owner SHANDONG UNIV OF TECH
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