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A kind of preparation method of rhombohedral anhydrous magnesium carbonate

An anhydrous magnesium carbonate, rhombohedral technology, applied in the direction of magnesium carbonate and the like, can solve the problems affecting the processing technology performance and product use performance, increasing the production cost, affecting the purity of the product, etc., and achieving easy control of production conditions, low production cost, Complete effect of crystal morphology

Active Publication Date: 2021-11-09
SHANDONG UNIV OF TECH
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  • Summary
  • 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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  • A kind of preparation method of rhombohedral anhydrous magnesium carbonate
  • A kind of preparation method of rhombohedral anhydrous magnesium carbonate

Examples

Experimental program
Comparison scheme
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 molar ratio of O is 1:8 by adding CH 4 N 2 O, stirred to obtain a mixed solution;

[0022] (2) MgCl 2 ·6H 2 O and CH 4 N 2 The mixed solution prepared by O is heated to carry out the pre-synthesis reaction, the reaction temperature is 95°C, and the reaction time is 1h;

[0023] (3) Move 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 150°C, and the reaction time is 2h;

[0024] (4) After the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain rhombohedral anhydrous magnesium carbonate. 25-30 μm.

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 molar ratio of O is 1:8 by adding CH 4 N 2 O, stirred to obtain a mixed solution;

[0027] (2) MgCl 2 ·6H 2 O and CH 4 N 2 The mixed solution prepared by O is heated to carry out the pre-synthesis reaction, the reaction temperature is 90°C, and the reaction time is 2h;

[0028] (3) Move 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 140°C, and the reaction time is 4h;

[0029] (4) After the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain rhombohedral anhydrous magnesium carbonate; anhydrous magnesium carbonate belongs to the trigonal crystal system, the side length of each rhomboid is 20-25 μm, and the rhombohe...

Embodiment 3

[0031] (1) MgCl 2 ·6H 2Add 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 molar ratio of O is 1:8 by adding CH 4 N 2 O, stirred to obtain a mixed solution;

[0032] (2) MgCl 2 ·6H 2 O and CH 4 N 2 The mixed solution prepared by O is heated to carry out the pre-synthesis reaction, the reaction temperature is 80°C, and the reaction time is 2h;

[0033] (3) Move 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;

[0034] (4) After the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain rhombohedral anhydrous magnesium carbonate; anhydrous magnesium carbonate belongs to the trigonal crystal system, the side length of each rhomboid is 20-25 μm, and the rhombohe...

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Abstract

The invention provides a preparation method of rhombohedral anhydrous magnesium carbonate, which belongs to the technical field of new inorganic chemical materials, and is characterized in that the following steps are adopted: MgCl 2 ·6H 2 Add O into distilled water to prepare a solution with a certain concentration, and add CH at a certain molar ratio 4 N 2 O, stir to obtain a mixed solution; heat the configured mixed solution to carry out a pre-synthesis reaction, the reaction temperature is 80-95°C, and the reaction time is 1-2h; the mixed solution after the pre-synthesis reaction is moved to a tank with polytetrafluoroethylene Hydrothermal reaction in a lined stainless steel reactor, the temperature of the hydrothermal reaction is 140-150°C, and the reaction time is 2-4h; after the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain rhombohedral anhydrous magnesium carbonate; Anhydrous magnesium carbonate The rhombohedral anhydrous magnesium carbonate prepared in the present invention belongs to the trigonal crystal system, the side length of each rhomboid is 20-25 μm, and the rhombohedral particle size is 25-30 μm.

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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Patent Type & Authority Patents(China)
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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