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A kind of preparation method of rhombohedral short column 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, 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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  • A kind of preparation method of rhombohedral short column anhydrous magnesium carbonate
  • A kind of preparation method of rhombohedral 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 molar ratio of O is 1:8 by adding CH 4 N 2 O, stirred to obtain a mixed solution;

[0023] (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;

[0024] (3) 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 moved 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;

[0025] (4) After the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain anhydrous magnesium carbonate with rhombohedral ...

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

[0028] (2) MgCl2 ·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;

[0029] (3) 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 moved 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;

[0030] (4) After the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain anhydrous magnesium carbonate with rhombohedral sh...

Embodiment 3

[0032] (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;

[0033] (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 85°C, and the reaction time is 2h;

[0034] (3) 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 moved 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;

[0035] (4) After the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain anhydrous magnesium carbonate with rhombohedral ...

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Abstract

The invention provides a preparation method of rhombohedral short column 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 transparent solution with a certain concentration, and add CH at a certain molar ratio 4 N 2 O, stirred to obtain a mixed solution; the mixed solution was heated to carry out a pre-synthesis reaction, the reaction temperature was 80-95°C, and the reaction time was 1-2h; the NH 3 ·H 2 O is slowly added dropwise in the mixed solution of pre-synthetic reaction, and the pH value of the mixed solution is adjusted to be 13; 150°C, the reaction time is 3‑4h; after the hydrothermal reaction is completed, the product is filtered and washed under negative pressure to obtain rhombohedral short column anhydrous magnesium carbonate; anhydrous magnesium carbonate belongs to the trigonal crystal system, and is polymerized by cylinder and rhombohedron The cross-section of the short column is circular, and the two ends of the column are three nearly quadrilateral flat crystal faces, the diameter of the column is 15-20 μm, and the length of the short column is 25-30 μm.

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 Patents(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