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A kind of preparation method of dirhombohedral 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, 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: 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 birhombohedral anhydrous magnesium carbonate crystals with a 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 dirhombohedral anhydrous magnesium carbonate
  • A kind of preparation method of dirhombohedral 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 0.2 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;

[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) Slowly add NaOH to the mixed solution of the pre-synthesis reaction, adjust the pH value of the mixed solution to 13; then move the mixed solution to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction, and the hydrothermal reaction The temperature is 160°C, and the reaction time is 4h;

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

Embodiment 2

[0027] (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;

[0028] (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;

[0029] (3) Slowly add NaOH to the mixed solution of the pre-synthesis reaction, adjust the pH value of the mixed solution to 13; then move the mixed solution to a stainless steel reactor with a polytetrafluoroethylene liner for hydrothermal reaction, and the hydrothermal reaction The temperature is 150°C, and the reaction time is 6h;

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

Embodiment 3

[0032] (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 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) Slowly add NaOH to the mixed solution of the pre-synthesis reaction, adjust the pH value of the mixed solution to 13; then move the mixed solution to a stainless steel reactor with a polytetrafluoroethylene lining for hydrothermal reaction, The temperature is 155°C, and the reaction time is 5h;

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

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Abstract

The invention provides a preparation method of double 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: 2 ·6H 2 O is added to distilled water to prepare a transparent solution with a certain concentration, and CH is added according to a certain molar ratio. 4 N 2 O, stir to obtain a mixed solution; heat the mixed solution to carry out a pre-synthesis reaction, the reaction temperature is 80-95 ℃, and the reaction time is 1-2h; slowly add NaOH to the mixed solution of the pre-synthesis reaction, and adjust the pH of the mixed solution to 13 ; Move the mixed solution to a stainless steel reactor with a polytetrafluoroethylene lining for hydrothermal reaction, the temperature of the hydrothermal reaction is 150-160 ° C, and the reaction time is 4-6 h; After the hydrothermal reaction is completed, the product is negatively charged. Press filtering and washing to obtain double rhombohedral anhydrous magnesium carbonate; the double rhombohedral anhydrous magnesium carbonate belongs to the trigonal crystal system, and the crystal is formed by the polymerization of two rhombohedrons, and the crystal diameter is 10-20 μm and the length is 20-35 μm.

Description

technical field [0001] The invention relates to a preparation method of dirhombohedral 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 met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F5/24
CPCC01F5/24C01P2004/30C01P2004/61
Inventor 李国昌李成峰孙海滨
Owner SHANDONG UNIV OF TECH
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