Preparation method of barium carbonate powder

A technology of barium carbonate and powder, which is applied in the direction of calcium carbonate/strontium/barium, bulk chemical production, nanotechnology, etc., and can solve the problem of difficult large-scale industrial production of barium carbonate, easy bonding or agglomeration of particles, poor particle uniformity, etc. problems, to achieve the effect of simple and easy-to-operate preparation method, good dispersibility, and little solvent pollution

Inactive Publication Date: 2012-04-18
FUDAN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] There are many methods for preparing and controlling barium carbonate crystals reported at present, such as liquid phase precipitation method, microemulsion method, low temperature solid phase synthesis method, sonochemical method, microwave synthesis method, high gravity method, etc. These methods have the disadvantages of poor particle uniformity, Problems such as the use of organic solvents, complex process control, harsh reaction conditions, and easy bonding or agglomeration of particles make it difficult to achieve large-scale industrial production of barium carbonate.

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  • Preparation method of barium carbonate powder
  • Preparation method of barium carbonate powder
  • Preparation method of barium carbonate powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] All glass instruments used in the experiment were pretreated as follows: firstly, they were sonicated in ethanol for 30 minutes, and then they were taken out and rinsed with deionized water. Put it into the mixed solvent of concentrated nitric acid / hydrogen peroxide / water according to the volume ratio of 1:1:1 and soak for 2 days, take it out, wash it with acetone, and dry it at room temperature. Prepare 0.1 g / L sodium carboxymethyl cellulose (molecular weight is 7×10 5 g / mol) aqueous solution 50 milliliters, then add a certain amount of barium hydroxide and be mixed with the barium hydroxide solution of 0.025 mol / liter, adjust the pH of solution to 8. Transfer the beaker containing the solution to a stainless steel autoclave, seal and evacuate until the vacuum degree is less than 10Pa. The temperature of the reaction oil bath was controlled to be 35° C., and carbon dioxide gas was slowly charged to make the pressure in the kettle be 4.5 MPa, and the reaction was maint...

Embodiment 2

[0034] The glass instrument processing method is the same as in Example 1. The method of operation of the experiment is also basically the same as in Example 1, except that sodium carboxymethylcellulose (molecular weight is 9 × 10 4 (gram / mole) aqueous solution concentration is 2 grams / liter, and the concentration of barium hydroxide solution is 0.03 mole / liter, and the pH of solution is 8.5, and reaction oil bath temperature is 50 ℃, and pressure in still is 6.5 MPa, and reaction time is 60 minute. Finally, the drying method for the obtained barium carbonate powder is as follows: drying at 40° C. for 10 hours under a vacuum degree of about 10 Pa. From figure 2It can be seen that the barium carbonate particles obtained in this embodiment are still a symmetrical dendritic structure bundled from the middle, but compared to the structure obtained in Example 1, the overall structure of the barium carbonate particles obtained in this embodiment The length is between 4-8 microns...

Embodiment 3

[0036] The glass instrument processing method is the same as in Example 1. The method of operation of the experiment is also basically the same as in Example 1, except that sodium carboxymethylcellulose (molecular weight is 9 × 10 4 (gram / mole) aqueous solution concentration is 10 grams / liter, and the concentration of barium hydroxide solution is 0.035 mole / liter, and the pH of solution is 7.5, and reaction oil bath temperature is 25 ℃, and still internal pressure is 3.5 MPa, reaction time 30 minute. Finally, the drying method for the obtained barium carbonate powder is as follows: drying at 25° C. for 24 hours under a vacuum degree of about 100 Pa. From image 3 It can be seen from the figure that the barium carbonate particles obtained in this example are almost all double-sphere structures, the diameter of the balls is between 500 nanometers and 1 micron, and the overall length is between 1-4 microns. It can be seen from an enlarged picture of double-sphere particles tha...

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Abstract

The invention, belonging to the technical field of inorganic salt materials, provides a preparation method of barium carbonate powder. The method comprises the following steps: selecting proper barium salt, adding a fresh prepared morphology regulator (water-soluble cellulose derivative), regulating the pH value to a proper value, using high pressure/supercritical carbon dioxide as a carbonic acid source (with certain temperature and pressure), reacting for different time to obtain a white turbid liquid; and separating and drying the white turbid liquid to obtain a required product. According to the invention, the batch production of barium carbonate powder with different morphologies (rodlike-type, dendritic-type, dumbbell-type, ball-type, symmetric-type and the like) and dimensions (500 nm-30 mu m) can be realized, the obtained barium carbonate product has good dispersibility and has a purity of more than 99.8 %; in addition, the method has the advantages of wide source of raw materials, low price, easy operation, little pollution of the used solvents, and no toxic and harmful effect, satisfies the requirement of green chemistry, and has the potential of large scale production.

Description

technical field [0001] The invention belongs to the technical field of inorganic salt materials, and in particular relates to a preparation method of barium carbonate powder. Background technique [0002] Barium carbonate is an important inorganic chemical raw material. As the barium carbonate powder with the largest production scale in barium salt products, it has great potential in the manufacture of glass, ceramics, coatings, microelectronic devices, magnetic materials, superconductor materials and other barium salts. the use of. The particle size and crystallization properties of barium carbonate particles will greatly affect its application in the above fields. Therefore, providing barium carbonate powders with crystals of different shapes and good dispersibility is helpful for the selective synthesis of barium-based functional materials and process optimization. [0003] There are many methods for preparing and controlling barium carbonate crystals reported at presen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/18B82Y40/00
CPCY02P20/54
Inventor 沈丹萍李为武培怡
Owner FUDAN UNIV
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