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Water heat modification method for high dispersion magnesium hydroxide nanometer sheet

A technology of magnesium hydroxide and hydrothermal modification, applied in magnesium hydroxide and other directions, can solve the problems of environmental pollution, high cost, difficult industrial promotion, etc., and achieve the effects of easy industrial amplification, regular morphology and simple process

Inactive Publication Date: 2006-07-12
TSINGHUA UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

The direct precipitation method is to contain Mg 2+ Add inorganic alkali to the solution to precipitate magnesium hydroxide. The method is simple and easy; the uniform precipitation method uses hydrolysis reaction (such as alcohol salt hydrolysis, urea hydrolysis, etc.) to slowly precipitate the crystal-forming ions in the solution. The product produced by the method has high purity and uniform particle size distribution, but the yield is low; the particles produced by the supergravity method are fine, but the solid-liquid separation is difficult and the process consumes a lot of energy
The common disadvantage of the above methods is that the morphology and dispersion of magnesium hydroxide cannot be controlled, and the products are often irregularly aggregated, which makes the nano-characteristics of the material unable to play normally.
Hydrothermal modification of conventional agglomerated products (Xiang Lan, Jin Yongcheng, Wei Fei, Jin Yong, Preparation method of highly dispersed flaky magnesium hydroxide, CN 1401574A, 2003; Li Zhiqiang, Wu Qingliu, Xiang Lan, Wei Fei, Hydrothermal modification The impact of the conditions on the preparation of magnesium hydroxide flame retardant pilot test, Chemical Industry Journal, 2005, 56 (7): 1349-1354) or azeotropic distillation (Dai Yanlin, Hong Ling, Shi Liyi, precipitation-azeotropic distillation method Preparation of Nano Mg(OH) 2 , Shanghai University Journal (Natural Science Edition), 2003, 9 (5): 402-409) can improve the morphology or dispersibility of the product to a certain extent, but the former is mainly applicable to the fine magnesium hydroxide system with larger particle size , the effect on nano-magnesium hydroxide is not good, and the aggregate particle size is greater than 2 μm (Li Zhiqiang, Wu Qingliu, Xiang Lan, Wei Fei, The influence of hydrothermal modification conditions on the pilot study of the preparation of magnesium hydroxide flame retardant, Chemical Industry Journal, 2005 , 56(7): 1349-1354), the latter cost is high and the azeotropic solvent is easy to cause pollution to the environment, it is difficult to promote industrially

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  • Water heat modification method for high dispersion magnesium hydroxide nanometer sheet
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  • Water heat modification method for high dispersion magnesium hydroxide nanometer sheet

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preparation example Construction

[0020] The invention provides a substrate double-injection-hydrothermal modification preparation method of highly dispersed magnesium hydroxide nanosheets, using inorganic magnesium salt as raw material, inorganic alkali as precipitant, inorganic chloride salt as substrate solution, and substrate The double-injection-hydrothermal modification method improves the structure of the product, thereby preparing highly dispersed magnesium hydroxide nanosheets. The specific steps are as follows:

[0021] 1) Prepare an inorganic magnesium salt solution and an inorganic alkali solution with a concentration of 0.5 to 5 mol / liter, and add the above magnesium salt and alkali solution simultaneously at a rate of 1 to 10 ml / min at 10 to 80° C. -5mol / L inorganic chloride salt solution, control the molar ratio of magnesium salt, alkali and chloride salt to 1:1-3:1-3, continue to react for 0.5-2 hours after the feeding is completed, and obtain a white milky slurry;

[0022] 2) adding the above ...

Embodiment 1

[0027] Prepare 100 milliliters of 0.5 mol / liter magnesium sulfate solution, 100 milliliters of 0.5 mol / liter sodium hydroxide solution, and inject the above solution into 100 milliliters of 0.5 mol / liter at a speed of 1 milliliter / minute under stirring (300 rpm) conditions Sodium chloride solution, continue to react for 2 hours after the feeding is completed, and obtain a white milky slurry; add the above-mentioned slurry to a hydrothermal reactor, stir at a constant temperature of 250 ° C (150 rpm) for 6 hours, then cool, filter, wash, dry, Pulverize to obtain magnesium hydroxide nanosheets with an average thickness of 50nm, an average diameter of 300nm, an average aggregate particle diameter of 100nm and a purity of 98.5%.

Embodiment 2

[0029] Prepare 100 milliliters of 5 mol / liter magnesium nitrate solution, 100 milliliters of 5 mol / liter potassium hydroxide solution, inject 100 milliliters 5 mol / liter of above-mentioned solution simultaneously with the speed of 10 milliliters / minute under stirring (300 rpm) conditions Potassium chloride solution, continue to react for 0.5 hours after feeding, to obtain a white milky slurry; add the above slurry to a hydrothermal reactor, stir at 100 ° C (150 rpm) for 1 hour, then cool, filter, wash, dry, Pulverize to obtain magnesium hydroxide nanosheets with an average thickness of 10nm, an average diameter of 100nm, an average aggregate particle size of 600nm and a purity of 98.0%.

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Abstract

The invention discloses a substrate double-injection- hydrothermal modified method of high-dispersed magnesium hydroxide nanometer piece in the organic chemical technique domain, which is characterized by the following: adapting inorganic magnesium salt as raw material and inorganic alkaline as precipitant and inorganic chlorine salt as substrate solution; injecting the magnesium salt and inorganic chlorine salt solution at 10-80 deg.c; disposing the atmospheric product for 1-6 hours at 100-200 deg.c; improving the product structure through chlorine salt and hydrothermal environment to produce topographic regulation and good dispersion property magnesium hydroxide nanometer piece with 10-50nm even thickness, 30-300nm even diameter and 100 -600nm birdnesting particle size. The invention makes regular topographic, even grain size and good dispersing magnesium hydroxide nanometer piece, which is used in the plastic and rubber industry as high-property inorganic flame-proof brusque.

Description

technical field [0001] This patent relates to a new process for preparing highly dispersed magnesium hydroxide nanosheets, which belongs to the technical field of inorganic chemical industry. Background technique [0002] my country is a country with large magnesium resources, and magnesite and salt lake magnesium resources are very rich, but the research and development of magnesium salts are still in their infancy, and commercially available or exported products are all based on cheap primary products (such as magnesium sulfate, magnesium carbonate, common magnesium oxide, etc.) , ordinary magnesium hydroxide) in the majority, and advanced magnesium salt functional materials with high added value, high technical content, and rapid market demand growth (such as highly dispersed nano-magnesium salt materials, magnesium salt whiskers, etc.) are still in the laboratory research stage , limiting the high utilization of magnesium resources. [0003] As a basic inorganic chemical ...

Claims

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Application Information

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IPC IPC(8): C01F5/22
Inventor 向兰陈志航张英才林荣毅
Owner TSINGHUA UNIV
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