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Method for preparing nano alkaline-earth metal sulfate powder with different crystal morphology

An alkaline earth metal salt and alkaline earth metal technology, applied in the fields of calcium/strontium/barium sulfate, chemical instruments and methods, inorganic chemistry, etc. and other problems to achieve the effect of simple process

Inactive Publication Date: 2010-04-21
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problems that the powder prepared by the existing method has a large impurity content, a large particle size, and an irregular shape that are not conducive to application, the present invention provides a method for preparing nano-alkaline earth metal sulfate powders with different crystal shapes

Method used

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  • Method for preparing nano alkaline-earth metal sulfate powder with different crystal morphology
  • Method for preparing nano alkaline-earth metal sulfate powder with different crystal morphology
  • Method for preparing nano alkaline-earth metal sulfate powder with different crystal morphology

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specific Embodiment approach 1

[0006] Specific embodiment one: the method for preparing nano alkaline earth metal sulfate powders with different crystal shapes in this embodiment is completed by the following steps: one, at room temperature, utilize soluble alkaline earth metal salts and sulfates to prepare concentrations of 0.5~1.5mol / L alkaline earth metal salt solution and sulfate solution; 2. Under the condition of stirring the alkaline earth metal salt solution at a speed of 100~300rpm, add absolute ethanol into the alkaline earth metal salt solution and mix well, and the added anhydrous The volume of ethanol is 30-60% of the alkaline earth metal salt solution volume; 3. Under the stirring condition with 500~1000rpm speed, the sulfate solution is quickly added in the mixed solution, and the volume of the sulfate solution added is the 1 to 1.5 times the volume of the alkaline earth metal salt solution, add and continue to stir for 20 to 30 minutes, and the obtained precipitate is washed by centrifugal wa...

specific Embodiment approach 2

[0007] Specific embodiment two: the difference between this embodiment and specific embodiment one is: the alkaline earth metal salt in step one is a kind of alkaline earth metal chloride or alkaline earth metal nitrate, and the described alkaline earth metal nitrate is calcium nitrate, One or a combination of barium nitrate and strontium nitrate, and the alkaline earth metal chloride is one or a combination of calcium chloride, barium chloride, and strontium chloride.

[0008] When the alkaline earth metal salt is a combination of calcium nitrate and barium nitrate, or a combination of calcium chloride and barium chloride, the molar ratio of Ca to Ba is 2:3; when the alkaline earth metal salt is a combination of calcium nitrate and strontium nitrate When the alkaline earth metal salt is a composition of strontium nitrate and barium nitrate, or a composition of strontium chloride and barium chloride, the molar ratio of Ca to Sr is 7:3; At this time, the molar ratio of Sr to Ba...

specific Embodiment approach 3

[0009] Specific embodiment three: the difference between this embodiment and specific embodiment one is that the sulfate in step one is Na 2 SO 4 or K 2 SO 4 kind of. Others are the same as in the first embodiment.

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Abstract

A method for preparing nanometer alkaline earth metal sulfate powder of different crystal shapes belongs to the technical field of nanometer material preparation. The invention solves the problem thatthe powder prepared with the prior method has high impurity content and large particle diameters and is disadvantageous to application due to morphological irregularity. The invention comprises the following steps: preparing mixed solution with alkaline earth metal salt and anhydrous ethanol; adding the solution prepared with soluble sulfate to obtain precipitate; with centrifugal precipitation,washing repeatedly the precipitate to clear away impurity ions; continuing centrifugal washing with anhydrous ethanol; placing the precipitate obtained after the centrifugal washing in an autoclave and injecting ethanol; raising the temperature to 245-270 DEG C with a constant speed and adjusting the pressure in the autoclave to 4-8MPa; stabilizing the temperature for one to two hours and then discharging the ethanol slowly; purging the residual ethanol for 0.5 hour with nitrogen with a flow rate of 5-20ml / min; and taking dried powder out after the autoclave is cooled to room temperature. Themethod of the invention has simple process; the purity of the product is higher than 99.9 percent; the final morphology of the powder can be controlled.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to the preparation of nano alkaline earth metal sulfate powders with different crystal shapes by adopting a direct precipitation-supercritical fluid drying method. Background technique [0002] Alkaline earth metal sulfate is an important chemical product. With the continuous advancement of science and technology and the increasing development of information and biological industries, the market has higher and higher requirements for the quality of raw materials, especially in the fields of ceramics, coatings, papermaking and medicine where alkaline earth metal sulfates are widely used. The purity, particle size and uniformity requirements of the product are also getting higher and higher. Existing sulfate powders have a large impurity content of less than 97% and a purity of less than 97%. Most of their shapes are irregular granules, and the particle s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F11/46C01F13/00
Inventor 欧阳家虎李玉峰周玉
Owner HARBIN INST OF TECH
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