Preparation method of fibrous alkali magnesium sulfate whisker

A magnesium sulfate whisker and magnesium sulfate technology, applied in chemical instruments and methods, single crystal growth, crystal growth, etc., can solve the problems of difficulty in inhibiting the growth of fan-shaped whiskers, long hydrothermal reaction time, and low single-shot yield. Achieve the effect of realizing large-scale industrial production, easy large-scale industrial production, and reducing the cost of raw materials

Active Publication Date: 2014-05-14
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Claims
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Problems solved by technology

Chinese patent CN101319378A discloses a kind of preparation method of basic magnesium sulfate whisker, and this method is difficult to suppress the fan-shaped whisker growth
Lu Huigang controlled the synthesis of fibrous basic magnesium sulfate whiskers by optimizing the hydrothermal reaction conditions and adding EDTA. The range of reaction conditions is narrow, and the product quality is difficult to control during industrial operation; the hydrothermal reaction time is long, and the single output is low. EDTA causes problems such as difficulty in mother liquor circulation
[0003] In short, the predecessors have done a lot of work on fibrous basic magnesium sulfate whiskers, but there are problems such as complex process and uneven whisker morphology, which limit the further industrial application of related technologies

Method used

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  • Preparation method of fibrous alkali magnesium sulfate whisker
  • Preparation method of fibrous alkali magnesium sulfate whisker
  • Preparation method of fibrous alkali magnesium sulfate whisker

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Experimental program
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Embodiment 1

[0029] Prepare 1.0mol / L MgSO 4 ·7H 2 O solution 1.6 liters, add 98.5 grams of granular NaOH (MgSO 4 The molar ratio to NaOH is 0.65:1), aged at 25°C for 2 hours. Transfer the obtained slurry into a 2-liter reactor with a filling degree of 80%, add 0.55 g of seed crystals (particle size 0.2-2.0 μm), and stir evenly. The slurry was reacted at 130°C for 2 hours. After the reaction was completed, it was naturally cooled to room temperature. Filtrate, wash and dry the white suspension obtained after the hydrothermal reaction to obtain 152-type fibrous basic sulfuric acid with a length of 30-50 μm, a diameter of 0.2-0.5 μm, an aspect ratio of 60-200, and a main content of 98.0%. Magnesium whiskers.

Embodiment 2

[0031] Prepare 1.0mol / L MgSO 4 ·7H 2 O solution 1.6 liters, add 60.0 grams of granular NaOH (MgSO 4 The molar ratio to NaOH is 1:1), aged at 60°C for 24 hours. Move the obtained slurry into a 2-liter reactor with a filling degree of 75%, add 3.5 grams of seed crystals (0.2-2.0 μm in particle size), and stir evenly. The slurry was reacted at 180°C for 12 hours. After the reaction was completed, it was naturally cooled to room temperature. Filtrate, wash and dry the white suspension obtained after the hydrothermal reaction to obtain 152-type fibrous basic sulfuric acid with a length of 50-200 μm, a diameter of 0.5-1.0 μm, an aspect ratio of 50-400, and a main content of 98.7%. Magnesium whiskers.

Embodiment 3

[0033] Prepare 1.5mol / L MgSO 4 ·7H 2 O solution 1.0 L, add 92.3 g granular NaOH (MgSO 4 The molar ratio to NaOH is 0.65:1), aged at 100°C for 24 hours. Move the obtained slurry into a 2-liter reactor with a filling degree of 50%, add 4.0 grams of seed crystals (0.2-2.0 μm in particle size), and stir evenly. The slurry was reacted at 130°C for 12 hours. After the reaction was completed, it was naturally cooled to room temperature. Filtrate, wash and dry the white suspension obtained after the hydrothermal reaction to obtain 152-type fibrous basic sulfuric acid with a length of 50-200 μm, a diameter of 0.2-0.5 μm, an aspect ratio of 100-1000, and a main content of 98.9%. Magnesium whiskers.

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Abstract

The invention relates to the preparation field of chemical industrial materials, and particularly relates to a preparation method of a fibrous alkali magnesium sulfate whisker. The preparation method of the fibrous alkali magnesium sulfate whisker comprises the following steps: (1) preparing a magnesium sulfate solution by using MgSO4.7H2O, stirring and adding NaOH granular caustic soda, aging for 2-24 hours at the temperature of 25 to 100 DEG C to obtain a slurry; (2) transferring the slurry obtained in the step (1) into a hydrothermal reactor, wherein the filling degree is 50-80 percent, adding 0.5-5 percent of seed crystal according to the mass of the NaOH granular caustic soda, uniformly stirring, and reacting the slurry for 2-12 hours at the temperature of 130-180 DEG C; (3) cooling after finishing the reaction of the step (2), filtering, washing and drying a obtained white turbid liquid to obtain the fibrous alkali magnesium sulfate whisker. According to the preparation method, the seed crystal is added into the reaction slurry, alkali magnesium sulfate is easily subjected to nucleus formation growth, and the preparation concentration of the reaction slurry can be relatively high; the whisker nucleation time is reduced, and the whisker growth time also can be shortened.

Description

technical field [0001] The invention relates to the field of preparation of chemical materials, in particular to a method for preparing fibrous basic magnesium sulfate whiskers. Background technique [0002] Basic magnesium sulfate whisker is also known as magnesium oxysulfide whisker (referred to as MOS whisker), the chemical formula is MgSO 4 5Mg(OH) 2 ·3H 2 O or MgSO 4 5Mg(OH) 2 2H 2 O, the appearance is white powder, and it is a single needle-shaped or fan-shaped crystal under the microscope. It has the characteristics of high strength, low density and high elastic modulus. It can be used as a filling material for composite materials such as plastics, rubber, resins and ceramics to improve the matrix. mechanical properties. As a functional whisker, MOS can not only strengthen, but also be flame-retardant. It is a high-performance inorganic flame-retardant reinforcing material. To sum up, the preparation methods of basic magnesium sulfate whiskers mainly include th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/10C30B29/22C30B29/62
Inventor 乃学瑛王亚斌朱东海李列李武
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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