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Method for preparing long-rhombohedron and short-column rhombohedron anhydrous magnesium carbonate mixture

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

Active Publication Date: 2019-09-10
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, need to use organic additive, influence product purity and increase cost; Or use magnesium salt and precipitant hydrothermal method method, but requires higher synthesis stability and longer synthesis time
At present, there are few related research reports on the hydrothermal synthesis of rhombohedral and short prismatic rhombohedral anhydrous magnesium carbonate mixtures with single phase, good dispersion, uniform particle size, and complete crystal morphology without using organic solvents and chelating agents.

Method used

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  • Method for preparing long-rhombohedron and short-column rhombohedron anhydrous magnesium carbonate mixture
  • Method for preparing long-rhombohedron and short-column rhombohedron anhydrous magnesium carbonate mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (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;

[0023] (2) Slowly add NaOH to the mixed solution of the pre-synthesis reaction, adjust the pH value of the mixed solution to 11, and then move the mixed solution to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction. The temperature is 150°C, and the reaction time is 4h;

[0024] (3) After the hydrothermal reaction is completed, the product is filtered under negative pressure, washed and dried to obtain anhydrous magnesium carbonate.

[0025] Anhydrous magnesium carbonate is composed of two crystals with different s...

Embodiment 2

[0027] (1) MgCl 2 ·6H 2 Add O into distilled water to prepare a transparent solution with a concentration of 0.3 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 transparent solution; MgCl 2 ·6H 2 O and CH 4 N 2The solution prepared by O is heated to carry out pre-synthesis reaction, the reaction temperature is 90°C, and the reaction time is 1.5h;

[0028] (2) Slowly add NaOH to the mixed solution of the pre-synthesis reaction, adjust the pH value of the solution to 11, and then move the mixed solution to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction, the temperature of the hydrothermal reaction The temperature is 140°C, and the reaction time is 6h;

[0029] (3) After the hydrothermal reaction is completed, the product is filtered under negative pressure, washed and dried to obtain anhydrous magnesium carbonate.

Embodiment 3

[0031] (1) MgCl 2 ·6H 2 Add O into distilled water to prepare a transparent solution with a concentration of 0.2 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 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;

[0032] (2) Slowly add NaOH to the mixed solution of the pre-synthesis reaction, adjust the pH value of the solution to 11, and then move the mixed solution to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction, the temperature of the hydrothermal reaction The temperature is 145°C, and the reaction time is 5h;

[0033] (3) After the hydrothermal reaction is completed, the product is filtered under negative pressure, washed and dried to obtain anhydrous magnesium carbonate.

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Abstract

The invention provides a method for preparing a long-rhombohedron and short-column rhombohedron anhydrous magnesium carbonate mixture. The method is characterized by employing the following steps: adding MgCl2.6H2O and CH4N2O into distilled water according to a certain mass-mole ratio, so as to prepare a clear solution of a certain concentration; heating up the solution, and carrying out a pre-synthesis reaction for 1 to 2 hours at a reaction temperature of 80 DEG C to 95 DEG C; slowly adding NaOH into a pre-synthesis reacted mixed solution, and adjusting a pH value of the mixed solution to be11; transferring the mixed solution into a Teflon-lined stainless-steel reactor, and carrying out a hydrothermal reaction for 4 to 6 hours at a temperature of 140 DEG C to 150 DEG C; and subjecting aproduct to negative-pressure filtering, washing and baking after the hydrothermal reaction is completed, thereby obtaining anhydrous magnesium carbonate, wherein the anhydrous magnesium carbonate isformed through mixing two kinds of crystals of different morphologies, one kind of crystals are long rhombohedra, the other kind of crystals are short column rhombohedra, and both kinds belong to a trigonal crystal system, the long-rhombohedron anhydrous magnesium carbonate crystals have the diameter of 10 to 20 microns and the length of 25 to 50 microns, and the short-column-rhombohedron anhydrous magnesium carbonate crystals have the diameter of 15 to 20 microns and the length of 20 to 25 microns.

Description

technical field [0001] The invention relates to a preparation method of a mixture of anhydrous magnesium carbonate rhombohedron and short columnar rhombohedron, and 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/24
CPCC01F5/24C01P2002/72C01P2004/03C01P2004/11C01P2004/80
Inventor 李国昌李成峰孙海滨
Owner SHANDONG UNIV OF TECH
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