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Preparation method of rhombohedra short-column anhydrous magnesium carbonate

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, increasing production cost, affecting product purity, etc., and achieves easy control of production conditions, low production cost, The effect of complete crystal morphology

Active Publication Date: 2019-09-10
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, 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 short-column anhydrous magnesium carbonate 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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  • Preparation method of rhombohedra short-column anhydrous magnesium carbonate
  • Preparation method of rhombohedra short-column anhydrous magnesium carbonate

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) the NH 3 ·H 2 O was slowly added to the mixed solution of the pre-synthesis reaction, and the pH value of the mixed solution was adjusted to 13; then the mixed solution was transferred to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction, and the temperature of the hydrothermal reaction was 150°C , the reaction time is 3h;

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

Embodiment 2

[0027] (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 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 2The solution prepared by O is heated to carry out pre-synthesis reaction, the reaction temperature is 80°C, and the reaction time is 2h;

[0028] (2) the NH 3 ·H 2 O was slowly added to the mixed solution of the pre-synthesis reaction, and the pH value of the mixed solution was adjusted to 13; then the mixed solution was transferred to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction, and the temperature of the hydrothermal reaction was 140°C , the reaction time is 4h;

[0029] (3) After the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain rhombohedral short column 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 0.1 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 85°C, and the reaction time is 2h;

[0032] (2) the NH 3 ·H 2 O was slowly added to the mixed solution of the pre-synthesis reaction, and the pH value of the mixed solution was adjusted to 13; then the mixed solution was transferred to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction, and the temperature of the hydrothermal reaction was 145°C , the reaction time is 3h;

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

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Abstract

The invention provides a preparation method of a rhombohedra short-column anhydrous magnesium carbonate, and belongs to the technical field of inorganic chemical engineering materials. The preparationmethod is characterized by comprising the following steps: adding MgCl2.6H2O into distilled water to prepare a transparent solution with a certain concentration, adding CH4N2O according to a certainmass molar ratio, and carrying out stirring to obtain a transparent solution; heating the solution, and carrying out a pre-synthesis reaction, wherein the reaction temperature is 80-95 DEG C, and thereaction time is 1-2 hours; slowly dropwise adding NH3.H2O into a mixed solution of the pre-synthesis reaction, and adjusting the pH value of the mixed solution to be 13; transferring the mixed solution into a stainless-steel reaction kettle with a polytetrafluoroethylene lining for a hydrothermal reaction, wherein the hydrothermal reaction temperature is 140-150 DEG C, and the reaction time is 3-4 hours; and after the hydrothermal reaction is completed, carrying out negative-pressure filtration and washing on the product to obtain the rhombohedra short-column anhydrous magnesium carbonate. The anhydrous magnesium carbonate belongs to a trigonal crystal system and is formed by polymerizing a circular column and a rhombohedra, the cross section of the short column is circular, and each of two ends of the column are provided with three near-quadrilateral flat crystal surfaces, wherein the diameter of the circular column is 15-20 microns, and the length of the short column is 25-30 microns.

Description

technical field [0001] The invention relates to a preparation method of rhombohedral short column 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: carbon...

Claims

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Application Information

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