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Preparation method of spherical silica powder

A technology of spherical silicon micropowder and silicon source, applied in the direction of silicon oxide, silicon dioxide, etc., can solve the problems of wide particle size distribution, high equipment requirements, low spherical rate, etc., and achieve uniform particle size distribution, dense and smooth surface of the sphere, and flow good sex effect

Active Publication Date: 2021-08-31
刘亚
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Deflagration method: The submicron-sized spherical silica powder prepared by the VMC method using metal silicon has the characteristics of smooth surface and high amorphous content, but this method is currently monopolized by Japan and the United States, and strict blockade is carried out. Dust deflagration is formed, and there is a big safety hazard in the production process
[0007] Patent CN109455726A proposes to prepare spherical silicon micropowder by flame combustion method. The prepared spherical silicon micropowder has a wide particle size distribution and low sphericity. The particles must be classified to obtain uniformly distributed spherical silicon micropowder. Moreover, the flame has extremely high requirements on the equipment spheroidizing furnace. High, large investment in equipment and other issues
Patent CN107285322A proposes to use plasma process to prepare spherical silicon powder, and improve the process to prepare sub-nano spherical silicon powder. The spherical silicon prepared by plasma process has the advantages of good sphericity, high density and good fluidity, but the cost is high and the equipment High requirements, unable to industrialize mass production
In the patent CN102659123A, microemulsions are used to reverse prepare spherical silicon micropowder, water glass, ammonium salt, organic solvent and surfactant are used as raw materials, and condition parameters such as the ratio of organic solvent, dispersant, surfactant and water glass are controlled. Spherical microsilica powder has better sphericity, but the particle size distribution is wide, the particles are easy to agglomerate, and the surface has pits and other problems.

Method used

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Experimental program
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Effect test

Embodiment 1

[0031] A preparation method of spherical micro-silicon powder, which comprises the following steps:

[0032] (1) Add 20 g of sodium silicate into a membrane emulsification device with a membrane aperture of 10 μm to form a dispersed phase silicon source;

[0033] (2) Add 0.5 g of Tween-60 into 50 ml of deionized water and mix evenly to form a mixed solution;

[0034] (3) adding the dispersed-phase silicon source in step (1) to the mixed solution in step (2) under a pressure of 0.1 MPa to form a stable emulsion;

[0035] (4) Add 1g of ammonia water to the stable emulsion in step (3), stir for 45 minutes to obtain particle slurry;

[0036] (5) centrifuging the granular slurry obtained in step (4), and drying the obtained powder at 80° C. for 5 hours to obtain a dry powder;

[0037] (6) Calcining the dry powder obtained in step (5), the heating rate is 3 hours to 600° C., and the holding time is 8 hours to obtain spherical silicon oxide micropowder.

[0038] From figure 1 It ...

Embodiment 2

[0040] A preparation method of spherical micro-silicon powder, which comprises the following steps:

[0041] (1) Add 30 g of sodium silicate into a membrane emulsification device with a membrane aperture of 20 μm to form a dispersed phase silicon source;

[0042] (2) Add 0.5 g of Tween-60 into 50 parts of deionized water and mix evenly to form a mixed solution;

[0043] (3) adding the dispersed-phase silicon source in step (1) to the mixed solution in step (2) under a pressure of 0.1 MPa to form a stable emulsion;

[0044] (4) 1g of formic acid is added in the stable emulsion in step (3), stirred for 30 minutes to obtain particle slurry;

[0045] (5) centrifuging the granular slurry obtained in step (4), and drying the obtained powder at 80° C. for 5 hours to obtain a dry powder;

[0046] (6) Calcining the dry powder obtained in step (5), the heating rate is 3 hours to 600° C., and the holding time is 8 hours to obtain spherical silicon oxide micropowder.

[0047] The parti...

Embodiment 3

[0049] A preparation method of spherical micro-silicon powder, which comprises the following steps:

[0050] (1) Add 30 g of methyltrimethoxysilane into a membrane emulsification device with a membrane aperture of 30 μm to form a dispersed phase silicon source;

[0051] (2) Add 0.3 parts of Span-80 into 80 parts of deionized water and mix evenly to form a mixed solution;

[0052](3) adding the dispersed-phase silicon source in step (1) to the mixed solution in step (2) under a pressure of 0.05 MPa to form a stable emulsion;

[0053] (4) Add 1g of ammonia water to the stable emulsion in step (3), stir for 30 minutes to obtain particle slurry;

[0054] (5) centrifuging the particle slurry obtained in step (4), and drying the obtained powder at 100° C. for +6 hours to obtain a dry powder;

[0055] (6) Calcining the dry powder obtained in step (5), the heating rate is 4 hours to 500° C., and the holding time is 5 hours to obtain spherical silicon oxide micropowder.

[0056] The...

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Abstract

The invention discloses a preparation process of spherical silica powder, which comprises the following steps: forming a dispersed phase silicon source from a silicon source through membrane emulsification equipment, pressing the dispersed phase silicon source into deionized water containing an emulsifier under a certain pressure to form a stable emulsion, adding a curing agent into the stable emulsion to form particle slurry, and finally, carrying out solid-liquid separation, drying and calcining on the granular material to obtain the spherical silica powder. The preparation method disclosed by the invention has the characteristics of energy consumption saving, easily available raw materials, simplicity, high efficiency, mild reaction conditions, good repeatability and the like. The prepared spherical silica powder has the advantages that the sphericity rate is up to 98% or above, the spherical particle size distribution is uniform, the spherical particles are not agglomerated, the spherical surface is compact and smooth, the spherical silica powder is good in flowability, high in purity and the like, and the application prospect is wide.

Description

technical field [0001] The invention belongs to the field of inorganic material science, and in particular relates to a preparation method of spherical silicon micropowder. Background technique [0002] Spherical silica powder refers to the amorphous quartz powder material whose individual particles are spherical and the main component is silicon dioxide. The spherical silicon micropowder produced by our company using a special preparation process has the advantages of extremely high sphericity and spheroidization rate, high purity up to electronic grade, small particle size to submicron or nanometer level, uniform particle distribution, and no agglomeration. Widely used in CCL, EMC, electronic glue, plastic, film, polishing, special ceramics, ink coating and cosmetics and other fields. As a filler, spherical silica powder can greatly improve the rigidity, wear resistance, weather resistance, impact and compression resistance, tensile properties, flame resistance, arc resis...

Claims

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Application Information

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IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/03C01P2004/32C01P2004/61C01P2004/62
Inventor 刘亚
Owner 刘亚
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