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Preparation method of alkali type magnesium sulfate crystal whisker

A technology of magnesium sulfate whiskers and magnesium sulfate, applied in the direction of magnesium sulfate, chemical instruments and methods, single crystal growth, etc., can solve the problem of restricting the industrial production of basic magnesium sulfate whiskers, increasing process steps and raw material types, and being unsuitable for industrialization Production and other issues, to achieve the effect of saving resources, short preparation cycle, and easy process control

Inactive Publication Date: 2008-12-10
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The first type of method can grow more uniform and slender whiskers, but generally requires magnesium oxide to have higher activity and a certain particle size, which increases the process and difficulty of raw material preparation; the second type of method can also prepare Long fibrous whiskers with good shape are produced, but magnesium hydroxide raw materials with a certain particle size specification are also required, and magnesium hydroxide is not suitable for industrial production due to the difficulty in production and high cost
In addition, MgO and Mg(OH) 2 Slightly soluble, and MgSO 4 When the solution reacts, the rate is low, and the reaction conversion rate is low, and the purity is not high
The latter two methods belong to the direct hydrothermal synthesis of basic magnesium sulfate whiskers, which can avoid the shortcomings of the first two methods, but there are also many problems in the previous processes, such as some need to add various flocculants and dispersants and other additives, which undoubtedly increases the process and the types of raw materials, and some even need to filter and wash the magnesium hydroxide precipitate first, which is also a time-consuming and labor-intensive process.
And magnesium sulfate solution or sodium hydroxide solution concentration is lower in most technology, although can reduce reaction time, batch yield is little, is not suitable for suitability for suitability for industrialized production
In addition, MgSO 4 with Mg(OH) 2 Or the proportion of NaOH is too high, it will also reduce the batch yield and cause MgSO 4 massive waste of raw materials
For the above reasons, the industrialized production of basic magnesium sulfate whisker is limited

Method used

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  • Preparation method of alkali type magnesium sulfate crystal whisker
  • Preparation method of alkali type magnesium sulfate crystal whisker
  • Preparation method of alkali type magnesium sulfate crystal whisker

Examples

Experimental program
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Embodiment 1

[0024] Embodiment 1, with MgSO 4 ·7H 2 O prepared 1.0mol L -1 1.4L of magnesium sulfate solution, at room temperature, 56g of sodium hydroxide solid was added to it under stirring, and stirred continuously to make it fully react to form a uniform magnesium hydroxide sol-magnesium sulfate mixed precursor. Transfer 1.4L of the reaction slurry prepared at room temperature to a 2L autoclave with a filling degree of 70%, perform hydrothermal reaction at 170°C for 10 hours, the initial stirring speed is about 450rpm, and adjust to 300rpm after constant temperature reaction for 3h. After the reaction was completed, it was allowed to cool naturally, and the reaction product was filtered to separate the solid from the liquid, and washed with distilled water until there was no sulfate ion. The whisker filter cake was dried at 80° C. for 1 h to obtain 61 g of the product. The microscopic appearance of the product is (one-way or two-way) fan-shaped bundle of fibers, the length of the t...

Embodiment 2

[0025] Embodiment 2, with MgSO 4 ·7H 2 O prepared 2.5mol L -1 1.45 L of magnesium sulfate solution, at room temperature, 181 g of solid sodium hydroxide was added therein under stirring, and stirred continuously to make it fully react to form a uniform mixed precursor of magnesium hydroxide sol-magnesium sulfate. 1.6 L of the reaction slurry prepared at room temperature was transferred to a 2 L autoclave with a filling degree of 80%, and the hydrothermal reaction was carried out at 170° C. for 10 hours with a stirring intensity of 500 rpm. After the reaction was completed, it was allowed to cool naturally, and the reaction product was filtered to separate the solid from the liquid, and washed with distilled water until there was no sulfate ion. The whisker filter cake was dried at 80°C for 4 hours to obtain 195g of the product. The microscopic appearance of the product is partly fan-shaped bundle-like fibers, and partly dispersed whiskers are formed, with a diameter of abou...

Embodiment 3

[0026] Embodiment 3, with MgSO 4 ·7H 2 O prepared 2.0mol L -1 1.5 L of magnesium sulfate solution, at room temperature, add 150 g of solid sodium hydroxide to it under stirring, and keep stirring to make it fully react to form a uniform magnesium hydroxide sol-magnesium sulfate mixed precursor. 1.6L of the reaction slurry prepared at room temperature was transferred to a 2L autoclave with a filling degree of 80%, and the hydrothermal reaction was carried out at 170° C. for 10 hours, and the stirring intensity was 500-600 rpm. After the reaction was completed, it was allowed to cool naturally, and the reaction product was filtered to separate the solid from the liquid, and washed with distilled water until there was no sulfate ion. The whisker filter cake was dried at 80° C. for 4 hours to obtain 155 g of the product. The microscopic appearance of the product is (two-way or one-way) fan-shaped bundle fibers, the length of the two-way fan-shaped bundle fibers is about 40-50 μ...

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Abstract

The invention provides a method for preparing a basic magnesium sulfate whisker material, comprising the following steps that: a magnesium sulfate solution and sodium hydroxide solid are mixed according to a mol ratio of 0.6:1.0 to 1.0:1.5, the mixture is stirred at normal temperature so that an even magnesium hydroxide sol-magnesium sulfate solution reaction precursor is generated after the reaction; and the obtained reaction precursor is transferred into a hydrothermal reaction kettle to react at a temperature of between 130 and 180 DEG C for 6 to 20 hours, the solid and the fluid are separated after the reaction mixture is cooled naturally, the solid is pumped and filtered by distilled water and is washed until a sulfate ion is removed as well as is dried so that the basic magnesium sulfate whisker product is produced. The technology is easy to control, has simple operation, short preparation cycle, low production cost, low energy consumption and high quality of product, and is used to prepare the basic magnesium sulfate whisker product with high purity quotient, good quality and a yield coefficient more than 90 percent. The whisker product is identified to be pure phase by the X-ray diffraction. The method can obtain basic magnesium sulfate whiskers with different phases by controlling the reaction condition.

Description

technical field [0001] The invention belongs to the technical field of inorganic salt materials, and relates to a preparation method of a magnesium sulfate whisker material, in particular to a preparation method of a basic magnesium sulfate whisker material. Background technique [0002] Whiskers refer to single crystal fiber materials with a diameter of several microns and a length of tens of microns. It has the characteristics of large aspect ratio, no grain (edge) boundary, and the number of defects is smaller than that of polycrystalline. It is precisely because of this intrinsic integrity that whiskers, whose strength is not strictly limited by their surface integrity, are endowed with very tough and non-brittle properties compared to polycrystalline fibers and glass fibers. [0003] my country is rich in magnesium resources, but limited by technical and economic conditions, most of the current magnesium salt products are primary products with little technical content ...

Claims

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Application Information

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IPC IPC(8): C30B29/22C30B29/62C01F5/40
Inventor 边绍菊乃学瑛李洁魏明刘鑫李武
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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